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A preparation method of nitrogen-doped carbon nanotube-wrapped cobalt electrocatalytic oxygen reduction material

A technology of nitrogen-doped carbon and nanotubes, applied in chemical instruments and methods, physical/chemical process catalysts, circuits, etc., can solve problems such as poor stability and reduced catalytic activity, and achieve improved performance, high product purity, and improved activity Effect

Active Publication Date: 2018-04-27
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in practical applications, since the traditional preparation of carbon-supported transition metal / nitrogen-doped materials is to obtain the final catalyst material by simply stirring and mixing the precursors, evaporating to dryness, and heat treatment, this simple mixing method cannot effectively obtain the precursors. As a result, its catalytic activity cannot be fully exerted; in addition, during the pyrolysis process, transition metal salts are easily pyrolyzed into transition metal oxides in various valence states, resulting in reduced catalytic activity and poor stability.

Method used

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  • A preparation method of nitrogen-doped carbon nanotube-wrapped cobalt electrocatalytic oxygen reduction material
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  • A preparation method of nitrogen-doped carbon nanotube-wrapped cobalt electrocatalytic oxygen reduction material

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Embodiment 1

[0039] A method for preparing a nitrogen-doped carbon nanotube-wrapped cobalt electrocatalytic oxygen reduction material, comprising the following steps:

[0040] 1) Preparation of self-assembled melamine precursor: Weigh 9 mmol each of melamine and cobalt nitrate hexahydrate, 6 mmol of glucose, add 10 ml of water, after stirring evenly, adjust the pH to 2.5 with 1M hydrochloric acid, and continue stirring for 30 min. The product was centrifuged at 6000r / min, and the supernatant was removed and freeze-dried for use. The resulting product was pink in shape as a rod-like structure 4-10 μm long.

[0041] 2) Preparation of nitrogen-doped carbon nanotube-wrapped cobalt electrocatalytic oxygen reduction catalysts (Co-N-CNTs): put the self-assembled melamine precursor prepared in step 1) into a tube furnace, and raise the temperature to 550 °C under an argon atmosphere. ℃ for 3 hours, and then continue to heat up to 900 ℃ for 3 hours, the heating rate is 5 ℃ / min, the roasted product...

Embodiment 2

[0052] A method for preparing a nitrogen-doped carbon nanotube-wrapped cobalt electrocatalytic oxygen reduction material, comprising the following steps:

[0053] 1) Preparation of self-assembled melamine precursor: Weigh 9mmol melamine, 4.5mmol cobalt chloride hexahydrate and 3mmol glucose, add 10ml water, after stirring evenly, adjust the pH to 4 with 1M nitric acid, and continue stirring for 30min. The product was centrifuged at 6000r / min, and the supernatant was removed and freeze-dried for use.

[0054] 2) Preparation of nitrogen-doped carbon nanotube-wrapped cobalt nanoparticle hybrid material electrocatalytic oxygen reduction catalysts (Co-N-CNTs): put the self-assembled melamine precursor prepared in step 1) into a tube furnace, argon Under the atmosphere, the temperature was raised to 550 ° C for 3 h, and then the temperature was continuously raised to 800 ° C for 3 h at a rate of 2 ° C / min. The obtained roasted product was mixed with 0.1M H 2 SO 4 Mix and stir fo...

Embodiment 3

[0056] A method for preparing a nitrogen-doped carbon nanotube-wrapped cobalt electrocatalytic oxygen reduction material, comprising the following steps:

[0057] 1) Preparation of self-assembled melamine precursor: Weigh 9mmol melamine, 18mmol cobalt acetate tetrahydrate and 9mmol glucose, add 10ml water, after stirring evenly, adjust the pH to 5 with 1M nitric acid, and continue stirring for 30min. The product was centrifuged at 6000r / min, and the supernatant was removed and freeze-dried for use.

[0058] 2) Preparation of nitrogen-doped carbon nanotube-wrapped cobalt nanoparticle hybrid material electrocatalytic oxygen reduction catalysts (Co-N-CNTs): put the self-assembled melamine precursor prepared in step 1) into a tube furnace, argon Under the atmosphere, the temperature was raised to 550°C for 3h, and then the temperature was raised to 700°C for 3h, the heating rate was 10°C / min, and the obtained roasted product was mixed with 0.1M H 2 SO 4 Mix and stir for 1 h to r...

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Abstract

The invention discloses a preparation method of a cobalt electro-catalysis oxygen reduction material wrapping a nitrogen-doped carbon nanotube. The method includes the following steps of making melamine, cobalt nitrate hexahydrate and glucose react to obtain a self-assembled melamine precursor, and baking the self-assembled melamine precursor to obtain a cobalt nanoparticle hybrid material electro-catalysis oxygen reduction agent wrapping the nitrogen-doped carbon nanotube. In preparation of the precursor, a self-assembled body can be formed through the electrostatic interaction and the hydrogen-bond interaction by means of nitrate radicals and melamine under the acid condition, cobalt ions are adsorbed into the self-assembled body, ordered arrangement and assembly of materials in the high-temperature baking process are facilitated by the pre-assembled precursor, and therefore more catalysis active sites are exposed, and the improvement of the performance of a catalyst is facilitated.

Description

technical field [0001] The invention belongs to the technical field of materials and energy, and in particular relates to a preparation method of nitrogen-doped carbon nanotube-wrapped cobalt electrocatalytic oxygen reduction material. Background technique [0002] Fuel cells convert chemical energy directly into electrical energy by electrochemically reducing oxygen and oxidizing fuel to produce water as the only by-product, which is an efficient and green power generation technology. The kinetically slow cathode oxygen reduction reaction is an important factor limiting the performance of proton exchange membrane fuel cells (PEMFC) and direct methanol fuel cells (DMFC). Generally speaking, the oxygen reduction reaction performs energy conversion through two reaction pathways: (1) two-step two-electron transport pathway, the intermediate product is hydrogen peroxide; (2) four-electron transport pathway, water is the final reaction product, which This reaction pathway is mor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24H01M4/90
CPCH01M4/90Y02E60/50
Inventor 王宗花王晓涵赵凯夏建飞张菲菲龚世达
Owner QINGDAO UNIV
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