Preparation method of N/S-codoped carbon microspheres with high oxygen reduction catalytic activity

A catalytically active, co-doping technology, applied in electrical components, battery electrodes, circuits, etc., can solve the problems of no oxygen reduction catalytic electrochemical performance, no electrochemical performance, unfavorable large-scale synthesis, etc. The effect of strong oxygen reduction catalytic ability, strong tolerance and low cost

Active Publication Date: 2015-09-30
YANSHAN UNIV
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  • Abstract
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Problems solved by technology

However, the steps of these two preparation methods are relatively cumbersome, which is not conducive to large-scale synthesis
Qiu-Feng Lu et al. (Journal of Analytical and Applied Pyrolysis, 2012, 93: 147-152) obtained nitrogen-doped carbon hollow spheres by high-temperature pyrolysis of copolymers, and the material did not show electrochemical performance; Zheng Mingtao et al. (Acta Inorganic Chemistry, 2013, 29: 1391-1399) Using soluble starch as a carbon source, monodisperse sulfur-doped carbon microspheres with an average particle size of about 4 microns were prepared in one step by sulfur-assisted hydrothermal carbonization (550°C). However, the material did not exhibit electrochemical performance such as oxygen reduction catalysis.

Method used

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  • Preparation method of N/S-codoped carbon microspheres with high oxygen reduction catalytic activity
  • Preparation method of N/S-codoped carbon microspheres with high oxygen reduction catalytic activity
  • Preparation method of N/S-codoped carbon microspheres with high oxygen reduction catalytic activity

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Embodiment 1

[0025] In a nitrogen-protected glove box, add 0.2 g of cetyltrimethylammonium chloride, 0.5 g of analytically pure sublimed sulfur and 4 mL of ethylenediamine to 6 mL of toluene in sequence, stir for 2 minutes, and put the mixture into a volumetric Put it in a 15mL stainless steel reaction kettle, seal it; then place the reaction kettle in a crucible boiler, heat it at 300°C for 6h, then wait for the reaction kettle to cool down to room temperature naturally, and take out the mixture. The above mixture was washed 4 times successively with absolute ethanol, dilute hydrochloric acid and distilled water, filtered, and then vacuum-dried at 60°C for 12 hours, and the obtained product and analytically pure potassium hydroxide solid were mixed uniformly at a weight percentage of 1:2, and then Put it in a box-type atmosphere furnace and activate it in an argon atmosphere at 500°C for 2 hours, wash the activated product with dilute hydrochloric acid and distilled water for 5 times, and ...

Embodiment 2

[0029] In a nitrogen-protected glove box, 1 g of cetyltrimethylammonium bromide, 0.5 g of analytically pure TMTD, and 4 mL of acetonitrile were sequentially added to 24 mL of toluene, stirred for 4 minutes, and the mixture was put into a 45 mL volume of stainless steel In the reaction kettle, seal it; then place the reaction kettle in a crucible boiler, heat at 400°C for 18h, then wait for the reaction kettle to cool down to room temperature naturally, and take out the mixture. The above mixture was washed 5 times successively with absolute ethanol, dilute hydrochloric acid and distilled water, filtered, and then vacuum-dried at 80°C for 10 h, and the obtained product and analytically pure potassium hydroxide solid were mixed uniformly in a weight percentage of 1:1, and then placed Activate in a box-type atmosphere furnace at 600°C in an argon atmosphere for 1 hour, wash the activated product with dilute hydrochloric acid and distilled water for 5 times, and then dry it in vacu...

Embodiment 3

[0032]In a nitrogen-protected glove box, 1.5 g of cetyltrimethylammonium bromide, 2 g of analytically pure thiourea and 4 mL of acetonitrile were sequentially added to 24 mL of xylene, stirred for 6 minutes, and the mixture was placed in a volume of 45 mL In a stainless steel reaction kettle, seal it; then place the reaction kettle in a crucible boiler, heat it at 500°C for 24h, then wait for the reaction kettle to cool down to room temperature naturally, and take out the mixture. The above mixture was washed 6 times successively with absolute ethanol, dilute hydrochloric acid and distilled water, filtered, and then vacuum-dried at 100°C for 6 h, and the obtained product and analytically pure potassium hydroxide solid were mixed uniformly at a weight percentage of 2:1, and then placed Activated in a box-type atmosphere furnace in an argon atmosphere at 800°C for 0.5h, washed the activated product with dilute hydrochloric acid and distilled water for 4 times, and then dried in v...

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Abstract

The invention provides a preparation method of N/S-codoped carbon microspheres with high oxygen reduction catalytic activity. The preparation method comprises the following steps: adding a carbon source, a nitrogen source, a sulfur source and an analytically pure surfactant into a stainless steel reaction kettle in sequence under nitrogen protection, stirring, sealing, heating in a crucible furnace, and taking out a mixture when the reaction kettle is cooled naturally to room temperature; washing and filtering the mixture; drying obtained powder in a vacuum drying oven; uniformly mixing an obtained product with analytically pure potassium hydroxide powder, activating in an argon atmosphere; washing with distilled water; and finally, drying in vacuum in the vacuum drying oven. The preparation method has the advantages of simple process, mild reaction condition, high repeatability and low cost; in an alkaline environment, the generated product has excellent oxygen reduction catalytic property, is relatively high in catalytic activity, good in stability and relatively good in tolerance to methyl alcohol and carbon monoxide and has huge application potential on the aspect of fuel cell catalysts.

Description

technical field [0001] The invention relates to a preparation method of a fuel cell catalyst. Background technique [0002] With the development of society, human beings' demand for energy is increasing, and the energy crisis worldwide is gradually becoming prominent. As a clean, stable and efficient new energy source, fuel cells have been highly valued by people and are the focus of the new energy field. One of the directions of development. However, the energy conversion efficiency of fuel cells is severely constrained by the kinetics of the oxygen reduction reaction. Platinum and its alloys are by far the most efficient and widely used cathode catalysts for fuel cells. However, platinum-based catalysts also have some disadvantages that cannot be ignored. Platinum reserves are scarce in nature, so the cost has been high. In addition, platinum-based catalysts are less stable and less tolerant to carbon monoxide and methanol. These disadvantages greatly limit its practi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/88
CPCH01M4/8825Y02E60/50
Inventor 高发明张俊川周军双王栋尹航刘磊
Owner YANSHAN UNIV
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