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Nitrogen-doped graphene/nitrogen-doped carbon nanotube/tricobalt tetraoxide composite paper and preparation method thereof

A nitrogen-doped graphene and cobalt tetroxide technology is applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., to achieve good application prospects, enhanced ORR catalytic performance, and easy operation.

Inactive Publication Date: 2014-01-01
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In addition, most of the currently reported ORR catalysts are powder materials. In order to prepare the powder materials into a uniform dispersion when preparing the working electrode, long-term ultrasonic treatment is required.

Method used

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  • Nitrogen-doped graphene/nitrogen-doped carbon nanotube/tricobalt tetraoxide composite paper and preparation method thereof
  • Nitrogen-doped graphene/nitrogen-doped carbon nanotube/tricobalt tetraoxide composite paper and preparation method thereof
  • Nitrogen-doped graphene/nitrogen-doped carbon nanotube/tricobalt tetraoxide composite paper and preparation method thereof

Examples

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preparation example Construction

[0042] The invention provides a preparation method of nitrogen-doped graphene / nitrogen-doped carbon nanotube / cobalt tetroxide composite paper, comprising the following steps:

[0043] a. Provide graphene oxide dispersion;

[0044] This step a specifically includes the following steps:

[0045] a1. Pour a strong acid such as concentrated sulfuric acid into the mixture of graphite flakes and sodium nitrate, and stir to obtain a dispersion; the mass ratio of graphite flakes to sodium nitrate is preferably 4:3.

[0046] a2. Slowly add a strong oxidant such as potassium permanganate to the a1 dispersion, stir for about 20h, and place it for 2-8 days, preferably 5 days; the mass ratio of graphite flakes to potassium permanganate is preferably 1:3-1: 5.

[0047] a3. Add deionized water and hydrogen peroxide in sequence to a2; the ratio of hydrogen peroxide to potassium permanganate is about 5:2.

[0048] a4. The graphene oxide dispersion is obtained after repeated centrifugal wash...

Embodiment 1

[0072] (1) Preparation of graphene oxide dispersion: weigh 5.0 grams of graphite flakes and 3.75 grams of NaNO 3 Put it in a 1-liter beaker, turn on the mechanical stirring, and slowly add 150 ml of concentrated sulfuric acid (98%); after stirring for half an hour, add 20 grams of KMnO 4 Add to the above dispersion within half an hour; continue to stir for about 20 hours, because the viscosity of the reactant increases, the electric stirrer fails, stop stirring; after standing for 5 days (during the period, the reactant is occasionally stirred manually), slowly add 500 ml of deionized Water (stir while adding), stir well and slowly add 30 ml H 2 o 2 , to generate a bright yellow suspension; centrifuge the suspension, pour off the supernatant, keep the lower layer of precipitate, then add water to disperse the precipitate, repeat this process three times, wash away the residual metal ions; then, add water to disperse the obtained precipitate, centrifuge , collect the upper la...

Embodiment 2

[0078] Repeat Example 1, with the following differences: when preparing the graphene oxide / carbon nanotube composite paper containing cobalt ions, add 0.1 milliliter of 1 mol / liter cobalt nitrate aqueous solution. The nitrogen-doped graphene / nitrogen-doped carbon nanotube / cobalt tetroxide composite paper was observed with a field emission scanning electron microscope, and the result was similar to Example 1. The ORR electrocatalytic performance test was carried out on the nitrogen-doped graphene / nitrogen-doped carbon nanotube / cobalt oxide composite paper, the starting potential was about -0.06V, and the current density at -0.9V was -4.22mAcm -2 . The results show that the ORR electrocatalytic performance of nitrogen-doped graphene / nitrogen-doped carbon nanotubes / cobalt tetroxide composite paper described in Example 2 is lower than that of nitrogen-doped graphene / nitrogen-doped carbon nanotubes / cobalt tetroxide described in Example 1 Composite paper.

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Abstract

The invention provides a preparation method of nitrogen-doped graphene / nitrogen-doped carbon nanotube / tricobalt tetraoxide composite paper, which comprises the following steps: a) preparing a graphene oxide dispersion solution; b) preparing an oxidized carbon nanotube dispersion solution; c) mixing the graphene oxide dispersion solution and oxidized carbon nanotube dispersion solution with a cobalt nitrate water solution to obtain a slurry, applying the slurry onto a substrate, and drying to obtain the cobalt-ion-containing graphene oxide / oxidized carbon nanotube composite paper; and d) immersing the cobalt-ion-containing graphene oxide / oxidized carbon nanotube composite paper in an ammonia water solution, and carrying out hydrothermal reaction to obtain the final nitrogen-doped graphene / nitrogen-doped carbon nanotube / tricobalt tetraoxide composite paper. The method is simple to operate and mild in reaction conditions, can implement large-scale preparation of soft composite paper with favorable ORR catalytic property, and has favorable application prospects in the field of electrocatalysis.

Description

technical field [0001] The invention belongs to the technical field of nanomaterials, and more specifically relates to a nitrogen-doped graphene / nitrogen-doped carbon nanotube / cobalt tetroxide composite paper and a preparation method thereof. Background technique [0002] Cathodic oxygen reduction reaction (ORR) electrocatalysts are one of the key components in fuel cells and other electrochemical devices. The development of efficient ORR electrocatalysts plays a crucial role in the commercialization of fuel cells. Platinum-based materials have been studied for a long time due to their high catalytic activity. However, platinum is expensive, very sensitive to methanol and CO, and has poor durability, which hinders the large-scale application of fuel cells. To overcome this obstacle, researchers have developed a variety of ORR catalysts, such as perovskite, spinel, and nitrogen-doped carbon materials. However, the current catalyst materials still cannot fully meet the requi...

Claims

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Application Information

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IPC IPC(8): B01J27/24H01M4/90
CPCY02E60/50
Inventor 俞书宏李姗姗从怀萍
Owner UNIV OF SCI & TECH OF CHINA
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