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Preparation method of N-and-S-double-doped graphene/carbon nanotube aerogel

A technology of carbon nanotubes and graphene, which is applied in the field of preparation of N and S double-doped graphene/carbon nanotube aerogels, can solve the problems of effective specific surface area loss, lower specific capacitance, etc., and achieve enhanced reactivity and Conductivity, improvement of conductivity, and effect of improving electrochemical performance

Active Publication Date: 2018-11-16
福建宸琦新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This is because the strong van der Waals force and π-π stacking interactions between graphene layers make them easy to aggregate to form a graphitic structure, which leads to the loss of effective specific surface area and lowers its specific capacitance.

Method used

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  • Preparation method of N-and-S-double-doped graphene/carbon nanotube aerogel

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Embodiment 1

[0025] A preparation method of N and S double-doped graphene / carbon nanotube airgel, specifically comprising the following steps:

[0026] (1) Preparation of carboxylated carbon nanotubes: 1 g of multi-walled carbon nanotubes (MWCNTs) was added to 80 mL of concentrated HNO 3 , then condensed and refluxed in an oil bath at 120°C for 12 h, and the resulting black mixture was repeatedly washed and suction-filtered until pH = 7 to take the filter residue;

[0027] (2) Preparation of graphene oxide: After uniformly mixing graphite with concentrated sulfuric acid / concentrated phosphoric acid system (v / v=9:1), slowly add potassium permanganate, stir evenly for 0.5h, then stir in a 50°C water bath 12h, slowly add deionized water, and keep the temperature below 100°C, add 5wt% hydrogen peroxide dropwise, when the mixture turns golden yellow, add hydrochloric acid to wash, react for 5 minutes, wash with deionized water until neutral , and with BaCl 2 Detection of SO 4 2- residue, fo...

Embodiment 2

[0033] A preparation method of N and S double-doped graphene / carbon nanotube airgel, specifically comprising the following steps:

[0034] (1) Preparation of carboxylated carbon nanotubes: 1 g of multi-walled carbon nanotubes (MWCNTs) was added to 80 mL of concentrated HNO 3 , then condensed and refluxed in an oil bath at 120°C for 12 h, and the resulting black mixture was repeatedly washed and suction-filtered until pH = 7 to take the filter residue;

[0035] (2) Preparation of graphene oxide: After uniformly mixing graphite with concentrated sulfuric acid / concentrated phosphoric acid system (v / v=9:1), slowly add potassium permanganate, stir evenly for 0.5h, then stir in a 50°C water bath 12h, slowly add deionized water, and keep the temperature below 100°C, add 5wt% hydrogen peroxide dropwise, when the mixture turns golden yellow, add hydrochloric acid to wash, react for 5 minutes, wash with deionized water until neutral , and with BaCl 2 Detection of SO 4 2- residue, fo...

Embodiment 3

[0041] A preparation method of N and S double-doped graphene / carbon nanotube airgel, specifically comprising the following steps:

[0042] (1) Preparation of carboxylated carbon nanotubes: 1 g of multi-walled carbon nanotubes (MWCNTs) was added to 80 mL of concentrated HNO 3 , then condensed and refluxed in an oil bath at 120°C for 12 h, and the resulting black mixture was repeatedly washed and suction-filtered until pH = 7 to take the filter residue;

[0043] (2) Preparation of graphene oxide: After uniformly mixing graphite with concentrated sulfuric acid / concentrated phosphoric acid system (v / v=9:1), slowly add potassium permanganate, stir evenly for 0.5h, then stir in a 50°C water bath 12h, slowly add deionized water, and keep the temperature below 100°C, add 5wt% hydrogen peroxide dropwise, when the mixture turns golden yellow, add hydrochloric acid to wash, react for 5 minutes, wash with deionized water until neutral , and with BaCl 2 Detection of SO 4 2- residue, foll...

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Abstract

The invention discloses a preparation method of N-and-S-double-doped graphene / carbon nanotube aerogel and belongs to the technical field of preparation of an electrode material. The method is characterized by, to begin with, mixing carboxylated carbon nanotubes with graphene oxide, then, adding deionized water, and carrying out ultrasonic uniformly mixing to obtain a mixed solution; adding pyrroleand thiophene into the mixed solution, and carrying out first hydrothermal reaction to obtain hydrogel; adding the obtained hydrogel into a 2M KNO3 solution, carrying out secondary hydrothermal reaction, cooling to the room temperature, and then, carrying out filtering, washing and freeze drying; and carrying out thermal cracking on the product obtained after freeze drying in argon atmosphere toobtain the N-and-S-double-doped graphene / carbon nanotube aerogel. The graphene aerogel is doped with N and S, wherein the N and S double doping can further enhance reactivity and conductivity of the carbon material; compared with a single N or S doped material, the N-and-S-double-doped material introduces more active sites, thereby improving electrochemical performance thereof; and the N-and-S-double-doped graphene / carbon nanotube aerogel is expected to be used in electrode materials of supercapacitors.

Description

technical field [0001] The invention belongs to the technical field of electrode material preparation, and in particular relates to a preparation method of N and S double-doped graphene / carbon nanotube airgel. Background technique [0002] Among all carbon materials, such as carbon nanotubes, nanofibers, porous carbon, hollow nanospheres, carbon capsules, graphene nanosheets, graphene nanoribbons and their composites, graphene is superior due to its extraordinary electronic and mechanical properties. on other carbon materials. Although graphene has made considerable progress in supercapacitors, the performance is still not satisfactory. This is because the strong van der Waals force and π-π stacking interactions between graphene layers make them easy to aggregate to form a graphitic structure, which leads to the loss of effective specific surface area and lowers its specific capacitance. Therefore, in order to fully utilize the electrochemical properties of graphene, its s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01G11/24H01G11/30H01G11/36H01G11/38H01G11/86C01B32/184C01B32/168
CPCC01B32/168C01B32/184H01G11/24H01G11/30H01G11/36H01G11/38H01G11/86Y02E60/13
Inventor 郑玉婴周珺
Owner 福建宸琦新材料科技有限公司