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Iron nitride/nitrogen-doped graphene aerogel as well as preparation method and application thereof

A technology of nitrogen-doped graphene and graphene airgel, which is applied in chemical instruments and methods, chemical/physical processes, electrical components, etc., can solve the problem of low catalytic activity, achieve excellent performance, low cost, and superior stability and the effect of methanol oxidation resistance

Active Publication Date: 2014-04-16
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in order to obtain a current density similar to noble metal-doped graphene such as Pt / C catalysts, the loading capacity of these catalysts is usually several times that of Pt / C, and the catalytic activity is low under equal mass conditions.

Method used

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  • Iron nitride/nitrogen-doped graphene aerogel as well as preparation method and application thereof
  • Iron nitride/nitrogen-doped graphene aerogel as well as preparation method and application thereof
  • Iron nitride/nitrogen-doped graphene aerogel as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0040] 1. Preparation of graphite oxide:

[0041] In the present embodiment, graphite oxide is prepared by the following method: 1g graphite powder, 0.5g NaNO 3 And 23mL of concentrated sulfuric acid were added to a 250mL round bottom flask and stirred at room temperature for 24h.

[0042] Next, move the round-bottomed flask into an ice-water bath, and slowly add 3g of KMnO4 under vigorous stirring; deionized water, and then stirred for 15 min; then added 140 mL of water for dilution, and finally added 10 mL of 30% H 2 o 2 Stir for 10 min to end the reaction, and obtain a bright yellow suspension containing graphite oxide.

[0043] The above bright yellow suspension was centrifuged, the precipitate was washed twice with 10% HCl solution by volume, once with deionized water, centrifuged again, the precipitate was collected and dried in an oven at 70°C. The graphite oxide product was collected as a feedstock for subsequent steps.

[0044] 2. Preparation of iron nitride / nitr...

Embodiment 2

[0053] The graphite oxide prepared in Example 1 was used to prepare the iron nitride / nitrogen-doped graphene airgel, and the following examples were the same.

[0054] Disperse 24mg of graphite oxide and 24mg of ferrous phthalocyanine in 4mL of deionized water, and use ultrasonic dispersion to make it into a stable suspension to obtain a mixed solution;

[0055] Then transfer the mixed solution to a 20mL reaction kettle, add 12mL deionized water to make the graphite oxide concentration 1.5mg / mL, the mixed solution accounts for 80% of the reaction kettle volume, and carry out hydrothermal reaction at 200°C for 12h. Obtain hydrothermal reaction product;

[0056] The above hydrothermal reaction product was dried by freeze-drying method, and annealed at 700° C. for 3 hours in an ammonia atmosphere to obtain iron nitride / nitrogen-doped graphene airgel.

[0057] The obtained iron nitride / nitrogen-doped graphene airgel was characterized by TEM and SEM, and the results were the same ...

Embodiment 3

[0059] Disperse 24mg of graphite oxide and 24mg of ferrous phthalocyanine in 4mL of deionized water, and use ultrasonic dispersion to make it into a stable suspension to obtain a mixed solution;

[0060] Then transfer the mixed solution to a 20mL reaction kettle, add 12mL deionized water to make the graphite oxide concentration 1.5mg / mL, the mixed solution accounts for 80% of the reaction kettle volume, and carry out hydrothermal reaction at 180°C for 12h. Obtain hydrothermal reaction product;

[0061] The above hydrothermal reaction product was dried by freeze-drying method, and annealed at 750° C. for 3 hours in an ammonia atmosphere to obtain iron nitride / nitrogen-doped graphene airgel.

[0062] The obtained iron nitride / nitrogen-doped graphene airgel was characterized by TEM and SEM, and the results were the same as in Example 1. X-ray photoelectron spectroscopy analysis shows that the iron content is 2.01%, and the nitrogen content is 6.87%. This material is used as a ca...

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Abstract

The invention provides iron nitride / nitrogen-doped graphene aerogel as well as a preparation method and an application thereof. The iron nitride / nitrogen-doped graphene aerogel is three-dimensional nitrogen-doped graphene aerogel loaded with iron nitride nanoparticles. The invention further provides a preparation method of the iron nitride / nitrogen-doped graphene aerogel. The method comprises the following steps: dispersing graphite oxide and an organic iron compound in water according to a mass ratio of 1 to (0.5-4) to obtain a mixed solution of graphite oxide and the organic iron compound; adjusting the concentration of graphite oxide in the mixed solution to be 1.5-4mg / mL, and carrying out hydrothermal reaction at 180-220 DEG C for 10-14 hours to obtain a hydrothermal reaction product; drying the hydrothermal reaction product, and heating to 600-800 DEG C for 1-4 hours in an ammonia atmosphere to obtain the iron nitride / nitrogen-doped graphene aerogel. The iron nitride / nitrogen-doped graphene aerogel provided by the invention is excellent in catalytic oxidation reduction reaction capability and low in cost.

Description

technical field [0001] The invention provides an iron nitride / nitrogen-doped graphene airgel and a preparation method and application thereof, belonging to the field of material chemical synthesis. Background technique [0002] Graphene is composed of single layer sp 2 The hexagonal lattice formed by carbon atoms has attracted worldwide attention due to its unique properties since its discovery in 2004, and has been widely studied in many fields such as electronics, mechanics, and nanocatalysis. An important prerequisite for the application of graphene in energy conversion and storage is that its band gap, carrier concentration, and carrier polarity can be adjusted. Chemical doping is a practical way to adjust its performance without affecting the good conductivity of graphene. Feasible method. [0003] The application of this doped modified graphene material in the field of catalysts has also begun to attract attention. For example, graphene doped with metal nanoparticle...

Claims

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Application Information

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IPC IPC(8): B01J27/24H01M4/90
CPCY02E60/50
Inventor 侯仰龙尹涵
Owner PEKING UNIV
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