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Nitrogen-sulfur co-doped hollow hemispherical carbon-based material, preparation and application thereof

A technology of nitrogen-sulfur co-doping and carbon-based materials, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of incomplete exposure of reaction sites and poor redox electrocatalytic performance Good, small specific surface area, etc., to achieve good electrochemical oxygen reduction performance, abundant reaction sites, and controllable specific surface area

Inactive Publication Date: 2020-01-10
HUAZHONG UNIV OF SCI & TECH +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the above defects or improvement needs of the prior art, the present invention provides a nitrogen-sulfur co-doped hollow hemispherical carbon-based material, its preparation and application, which uses dopamine as a carbon source and a nitrogen source, and controls the orthosilicon The hemispherical silica obtained by the degree of hydrolysis of ethyl acetate was used as a template to prepare a nitrogen-sulfur co-doped hollow hemispherical carbon-based material, which was used as an oxygen reduction catalyst, thereby solving the existing nitrogen-sulfur co-doped spherical The technical problems of carbon-based materials with small specific surface area and incomplete exposure of reaction sites lead to poor redox electrocatalytic performance

Method used

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  • Nitrogen-sulfur co-doped hollow hemispherical carbon-based material, preparation and application thereof
  • Nitrogen-sulfur co-doped hollow hemispherical carbon-based material, preparation and application thereof
  • Nitrogen-sulfur co-doped hollow hemispherical carbon-based material, preparation and application thereof

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preparation example Construction

[0033] The invention provides a method for preparing a nitrogen-sulfur co-doped hollow hemispherical carbon-based material, comprising the following steps:

[0034] (1) Under an alkaline environment containing a solvent, partially hydrolyze ethyl orthosilicate to obtain a hemispherical silica template;

[0035] (2) Add dopamine hydrochloride to the system obtained in step (1) to obtain a hemispherical silica template, so that dopamine hydrochloride undergoes a polymerization reaction on the inner surface and outer surface of the hemispherical silica template obtained by partial hydrolysis, and solid-liquid after the reaction Separating and drying the obtained solid powder to obtain a dried sample;

[0036] (3) calcining the dried sample obtained in step (2) under an inert atmosphere to carbonize the polymer obtained by polymerizing dopamine hydrochloride to obtain a carbonized sample;

[0037] (4) removing the hemispherical silica template from the carbonized sample by acid e...

Embodiment 1

[0053] Mix 100ml of ethanol and 25ml of water in a 200ml beaker evenly, then take 5ml of ammonia water and add it to the mixed system of water and ethanol, mix evenly, then add 5ml of tetraethyl orthosilicate, stir for 10 minutes, add 300mg of dopamine hydrochloride, at 500 rpm React 24h under the stirring speed of / minute, obtain the compound of polydopamine and silicon dioxide, the obtained material is centrifugally washed and dried, then put into the tube furnace under the argon (flow rate is 120sccm) atmosphere and calcined, the heating rate is 5 Celsius / min, holding temperature 500°C, holding time 1h, then put the material into a mixed solvent of hydrofluoric acid and water with a volume ratio of 1:4, remove the acid for 5h, filter the obtained sample, dry it, and finally put the sample Anneal in a tube furnace under an argon (flow rate of 120 sccm) atmosphere, weigh the mass ratio of the sample to thiourea as 1:400, heat up at a rate of 10 degrees Celsius / min, hold at a ...

Embodiment 2

[0057] Mix 62.5ml of ethanol and 62.5ml of water in a 200ml beaker evenly, then take 10ml of ammonia water and add it to the mixed system of water and ethanol, mix evenly, then add 10ml of tetraethyl orthosilicate, stir for 10 minutes and then add 400mg of dopamine hydrochloride. React 6h under the stirring speed of 500 rev / mins, obtain the compound of polydopamine and silicon dioxide, the obtained material is centrifugally washed and dried, then put into the tube furnace under the argon (flow rate is 60sccm) atmosphere and calcined, the heating rate The temperature is 2 degrees Celsius / min, the holding temperature is 700 degrees Celsius, and the holding time is 4 hours. Next, the material is put into a mixed solvent of hydrofluoric acid and water with a volume ratio of 1:4, and the acid is removed for 2 hours. The obtained sample is suction filtered, dried, and finally The sample is annealed in a tube furnace under an argon (flow rate of 60 sccm) atmosphere, the mass ratio of ...

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Abstract

The invention belongs to the field of synthesis of carbon materials doped with impurity elements and the field of electrocatalytic oxygen reduction, and more particularly relates to a nitrogen-sulfurco-doped hollow hemispherical carbon-based material, preparation and application thereof. The invention provides the method for preparing the nitrogen-sulfur co-doped hollow hemispherical carbon-basedmaterial, and the method comprises the following steps of: controlling the hydrolysis degree of tetraethoxysilane to obtain hemispherical silicon dioxide microspheres serving as templates; polymerizing dopamine on the surface of the templates; carbonizing the obtained polymer; removing the templates; and finally doping sulfur in a gas phase to obtain the nitrogen-sulfur co-doped carbon-based material. The carbon-based material has the advantages of controllable specific surface area, controllable doping elements, good conductivity, good contact with electrolyte, rich reaction sites and the like, and has good electrochemical oxygen reduction performance when used as an oxygen reduction catalyst.

Description

technical field [0001] The invention belongs to the field of synthesis of heteroelement-doped carbon materials and the field of electrocatalytic oxygen reduction, and more specifically relates to a nitrogen-sulfur co-doped hollow hemispherical carbon-based material, its preparation and application. Background technique [0002] The oxygen reduction reaction plays a vital role in various energy conversion and storage systems, such as fuel cells and metal-air batteries. However, today's slow kinetics greatly limit the overall performance of these devices. To solve this problem, various catalysts have been extensively studied. Up to now, the precious metal catalyst platinum still has an unshakable position in terms of oxygen reduction performance. However, platinum-based materials have low earth abundance and are expensive. Therefore, in order to achieve the goal of practical application, metal-free carbon materials have shined in recent years because they are inexpensive an...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J35/00B01J35/02B01J37/00B01J37/08H01M4/90H01M4/96
CPCB01J27/24B01J37/084B01J37/082B01J37/0018H01M4/9091H01M4/96B01J35/33B01J35/50Y02E60/50
Inventor 王帅张翔宇肖菲肖军武池凯
Owner HUAZHONG UNIV OF SCI & TECH