Method for preparing nitrogen-doped graphene material in electrochemical stripping mode

A nitrogen-doped graphene, electrochemical technology, applied in chemical instruments and methods, graphene, inorganic chemistry, etc., can solve the problems of poor dispersion performance, toxic precursors, poor oxygen reduction activity, etc., to achieve high current density, Good water dispersibility and good methanol resistance

Inactive Publication Date: 2016-07-13
CHANGZHOU UNIV
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  • Abstract
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Problems solved by technology

[0003] Graphene plays an important role in the study of oxygen reduction reaction, but pure graphene is relatively inert and has poor oxygen reduction activity, but the catalytic activity of graphene for oxygen reduction reaction can be improved by doping nitrogen atoms
At present, the method of nitrogen doping is mainly heat treatment, but the nitrogen-doped graphene prepared by this method has the problems of toxic nitrogen precursors (such as NH3, pyridine) and poor dispersion in water.

Method used

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  • Method for preparing nitrogen-doped graphene material in electrochemical stripping mode
  • Method for preparing nitrogen-doped graphene material in electrochemical stripping mode
  • Method for preparing nitrogen-doped graphene material in electrochemical stripping mode

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Dissolve 0.56g of sodium sulfate, 2.5g of melamine, and 7.2mL of formaldehyde in 40mL of deionized water, adjust the pH of the solution to 6.0-9.0, use a graphite sheet as the positive electrode and a stainless steel sheet as the negative electrode, and apply 10V DC. After the expansion is completed, it is taken out and dried, and then calcined in a tube furnace at 650°C for 3 hours to obtain nitrogen-doped expanded graphite;

[0024] (2) Stripping the nitrogen-doped expanded graphite prepared in step (1) in a 0.5M ammonium sulfate solution with pH=6.0 to 9.0 by 10V direct current, suction filtering, washing and drying the stripped product to obtain the product. After XRD identification and SEM and TEM techniques, the product is electroexfoliated nitrogen-doped graphene.

Embodiment 2

[0026] (1) Dissolve 2.84g of sodium sulfate, 2.5g of dicyandiamide, and 3.6mL of formaldehyde in 40mL of deionized water, adjust the pH of the solution to 6.0-9.0, use a graphite sheet as the positive electrode and a stainless steel sheet as the negative electrode, and apply 2V direct current. After the expansion is completed, it is taken out and dried, and then calcined in a tube furnace at 750°C for 2 hours to obtain nitrogen-doped expanded graphite;

[0027] (2) Stripping the nitrogen-doped expanded graphite prepared in step (1) in a 0.1M ammonium sulfate solution with pH=6.0 to 9.0 by 10V direct current, suction filtering, washing and drying the stripped product to obtain the product. After XRD identification and SEM and TEM techniques, the product is electroexfoliated nitrogen-doped graphene. .

Embodiment 3

[0029] (1) Dissolve 5.6g of sodium sulfate, 2.5g of dicyandiamide, and 25.2mL of formaldehyde in 40mL of deionized water, adjust the pH of the solution to 6.0 to 9.0, use a graphite sheet as the positive electrode and a stainless steel sheet as the negative electrode, and apply 10V direct current. After the expansion is completed, it is taken out and dried, and then calcined in a tube furnace at 550°C for 6 hours to obtain nitrogen-doped expanded graphite;

[0030] (2) Stripping the nitrogen-doped expanded graphite prepared in step (1) in a 0.1M ammonium sulfate solution with a pH of 6.0 to 9.0 through 15V direct current, and suction filtering, washing and drying the stripped product to obtain the product. After XRD identification and SEM and TEM techniques, the product is electroexfoliated nitrogen-doped graphene.

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Abstract

The invention relates to a method for preparing a nitrogen-doped graphene material in an electrochemical stripping mode.The method includes the following specific steps that firstly, graphite is subjected to electrochemical stripping in a nitrogen-containing precursor; then, nitrogen-doped expanded graphite is prepared through thermal processing; finally, the nitrogen-doped expanded graphite is subjected to electrochemical stripping in inorganic electrolyte.The method has the advantages that the nitrogen-doped graphene prepared through the method is good in electrical conductivity and water dispersion performance; the preparation process is simple, convenient, easy to implement and free of pollution; when an electrode modified by the material is used as an electrocatalyst for a fuel cell cathode oxygen reduction reaction, the initial electric potential is low, current density is large, methanol resistance is good, and the electro-catalytic property of the material is close to that of a commercial Pt/C catalyst.

Description

technical field [0001] The invention relates to a method for preparing nitrogen-doped graphene, which belongs to the field of material preparation. Background technique [0002] Oxygen reduction reaction is a reaction that occurs at the fuel cell cathode. At present, Pt or Pt-based alloy catalysts are mainly used as fuel cell cathode catalysts. Due to the scarcity and high price of Pt resources, the battery cost is too high, which seriously hinders the commercialization of fuel cells. It is very meaningful to replace Pt with non-noble metal catalytic materials and carbon nanostructure (carbon nanotubes, graphene, etc.) materials containing doping elements (S, N, B) as fuel cell cathode catalysts. [0003] Graphene plays an important role in the study of oxygen reduction reaction, but pure graphene is relatively inert and has poor oxygen reduction activity, but the catalytic activity of graphene for oxygen reduction reaction can be improved by doping nitrogen atoms. At prese...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
CPCC01B2204/22C01P2002/72C01P2004/03C01P2004/04C01P2006/22
Inventor 秦勇晁磊袁杰储富强孔泳
Owner CHANGZHOU UNIV
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