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A kind of electrochemical preparation method of nitrogen-doped carbon material

A nitrogen-doped carbon, electrochemical technology, applied in electrodes, electrolysis components, electrolysis process and other directions, can solve the problems of harsh synthesis conditions, influence of nitrogen-doped carbon material performance, complicated steps, etc., achieve mild processing conditions, improve oxygen The effect of reducing catalytic performance and improving electrical conductivity

Active Publication Date: 2019-04-05
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In summary, the N atoms in the nitrogen-doped carbon materials synthesized by the template method mostly exist in the form of structural N, so nitrogen doping is more stable, but the steps are very complicated and high-temperature carbonization is required; chemical vapor deposition method synthesized The nitrogen-doped carbon material has a high N content, but its synthesis conditions are very harsh; the solvothermal method will introduce metal heteroatoms during the synthesis process. Although it is processed later, there will inevitably be residual metal atoms. It may affect the performance of nitrogen-doped carbon materials; the arc discharge method requires DC discharge treatment in an ammonia atmosphere; the treatment temperature of the heat treatment method is high, and other treatment methods have also been tried in different aspects, but nitrogen The doping process cannot avoid relatively harsh processing conditions

Method used

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  • A kind of electrochemical preparation method of nitrogen-doped carbon material
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  • A kind of electrochemical preparation method of nitrogen-doped carbon material

Examples

Experimental program
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Effect test

Embodiment 1

[0028] (1) Using commercial carbon fiber paper as a raw material, cut the carbon fiber paper into a rectangular sheet of 1cm×2cm, place it in a 1mol / L KOH solution, let it stand in a water bath at 60°C for 2h, and then ultrasonically treat it for 15 minutes to drive off the carbon fiber The air bubbles on the surface of the paper enable the carbon fiber paper to fully contact with the electrolyte;

[0029] (2) Clamp the processed carbon fiber paper rectangular sheet on the electrode holder, and wrap it with raw tape to ensure that the exposed area is 1cm 2 , the wound electrode clip is used as the working electrode, the platinum mesh electrode is used as the counter electrode, and the mercurous sulfate electrode is used as the reference electrode to form a three-electrode working system, which is fixed in the electrolytic cell;

[0030] (3) Configure a 3mol / L concentrated nitric acid solution as the electrolyte and add it to the electrolytic cell, so that the exposed part of t...

Embodiment 2

[0060] (1) Using commercial carbon fiber paper as a raw material, cut the carbon fiber paper into a rectangular sheet of 1cm×2cm, place it in a 1mol / L KOH solution, let it stand in a water bath at 60°C for 2h, and then ultrasonically treat it for 15 minutes to drive off the carbon fiber The air bubbles on the surface of the paper enable the carbon fiber paper to fully contact with the electrolyte;

[0061] (2) Clamp the processed carbon fiber paper rectangular sheet on the electrode holder, and wrap it with raw tape to ensure that the exposed area is 1cm 2 , the wound electrode clip is used as the working electrode, the platinum mesh electrode is used as the counter electrode, and the mercurous sulfate electrode is used as the reference electrode to form a three-electrode working system, which is fixed in the electrolytic cell;

[0062] (3) Configure a 4mol / L concentrated nitric acid solution as the electrolyte and add it to the electrolytic cell, so that the exposed part of t...

Embodiment 3

[0067] (1) Using graphene as a raw material, configure a 1 mg / ml graphene ethanol solution, and process it ultrasonically for 30 min;

[0068] (2) Polish the glassy carbon electrode, use a pipette gun, carefully move the prepared graphene solution to the surface of platinum carbon, and dry it naturally as a working electrode;

[0069] (2) Platinum grid electrode is used as counter electrode, and mercurous sulfate electrode is used as reference electrode to form a three-electrode working system, which is fixed in the electrolytic cell;

[0070] (3) Configure a 6mol / L concentrated nitric acid solution as the electrolyte and add it to the electrolytic cell so that the electrolyte is completely submerged on the surface of the platinum carbon electrode;

[0071] (4) Connect the electrochemical workstation, adopt the constant potential method, and conduct the electrochemical reaction at 1.20V vs. SSE (relative to the voltage under the saturated mercurous sulfate reference electrode)...

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Abstract

The invention provides an electrochemical preparing method for a nitrogen-doping carbon material. The electrochemical preparing method includes the steps that firstly, the carbon material is manufactured to be in a rectangular sheet shape and is clamped on an electrode clamp to serve as a work electrode, a platinum net electrode serves as a counter electrode, a mercurous sulfate electrode serves as a reference electrode, and a three-electrode work system is formed; a concentrated nitride acid solution of 2 mol / L to 14 mol / L serves as an electrolyte and is connected with an electrochemical work station, and the concentrated nitride acid solution is subjected to an electrochemical reaction through the electrochemical method; and after the electrochemical reaction is over, the work electrode is taken out, the carbon material is flushed through ultra-pure water 3-5 times and is then put into a vacuum drying tank, vacuum drying is conducted for 5 h to 12 h under the temperature ranging from 40 DEG C to 50 DEG C, and therefore the nitrogen-doping carbon material can be obtained. By means of the electrochemical preparing method, raw materials capable of being treated are wide, the treatment process is simple, the treatment conditions are moderate, the investment is small, the cost is low, nitrogen doping can be effectively conducted in the carbon material, the electric charge density of the carbon material is increased, and conductivity and oxygen reduction catalytic performance of the carbon materials are effectively improved.

Description

technical field [0001] The invention belongs to the technical field of inorganic advanced nanometer material preparation technology, and in particular relates to an electrochemical preparation method of nitrogen-doped carbon material. Background technique [0002] Carbon materials are currently the most widely used inorganic non-metallic materials, and have attracted much attention because of their excellent energy storage, adsorption, loading and catalytic properties. In order to expand the application range of carbon materials and improve the performance of carbon materials, researchers have carried out studies on the modification of carbon materials by heteroatom doping. The results show that among many elements, nitrogen has the most ideal effect in doping carbon materials. This is because the nitrogen element is located in group VA, adjacent to the carbon atom, and the atomic radius is close to that of the carbon atom, so the lattice distortion of the carbon material c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B1/00C25B1/04C25B11/12
CPCC25B1/00C25B11/043Y02E60/36
Inventor 张俊锋尹燕王庆法祝伟康张香文
Owner TIANJIN UNIV