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Preparation method of Fe/Fe3C nanoparticle-loaded porous nitrogen-doped carbon-based oxygen reduction catalyst

A nitrogen-doped carbon, nanoparticle technology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve problems such as loss of catalytic active sites, achieve excellent oxygen reduction performance, accelerate material The effect of transmission, high effective specific surface area

Active Publication Date: 2021-04-13
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, during the preparation process Fe, Fe 3 The self-agglomeration phenomenon of nanoparticles such as C will lead to the loss of catalytic active sites

Method used

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  • Preparation method of Fe/Fe3C nanoparticle-loaded porous nitrogen-doped carbon-based oxygen reduction catalyst
  • Preparation method of Fe/Fe3C nanoparticle-loaded porous nitrogen-doped carbon-based oxygen reduction catalyst
  • Preparation method of Fe/Fe3C nanoparticle-loaded porous nitrogen-doped carbon-based oxygen reduction catalyst

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Experimental program
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Effect test

Embodiment 1

[0027] Step S1: Dissolve 5g of melamine and 5mL of formaldehyde in 50mL of deionized water, place in a water bath at 60°C and stir for 30min to mix evenly, then add 1g of SiO 2 and 2 mL of glacial acetic acid, continued to stir at this temperature for 1 h, then stirred overnight at room temperature, centrifuged and dried to obtain material A1;

[0028]Step S2: Transfer material A1 to a nickel boat and place it in a tube furnace. In an inert gas atmosphere, first raise the temperature from room temperature to 300°C for 55 minutes and keep it for 60 minutes, then raise the temperature to 800°C at a heating rate of 5°C / min and Keep for 120min, then naturally cool to room temperature to obtain material B1;

[0029] Step S3: Transfer the material B1 to a 20 wt% hydrofluoric acid solution, soak it for 24 hours, wash it with high-purity water until neutral, and then dry it in an oven at 80°C for 12 hours to obtain the target product C1.

Embodiment 2

[0031] Step S1: Dissolve 5g of melamine and 5mL of formaldehyde in 50mL of deionized water, place in a water bath at 60°C and stir for 30min to mix evenly, then add 1g of SiO 2 , 0.5g iron acetylacetonate and 2mL glacial acetic acid, continue to stir at this temperature for 1h, then stir overnight at room temperature, obtain material A2 by centrifugation and drying:

[0032] Step S2: Transfer the material A2 to a nickel boat and place it in a tube furnace. In an inert gas atmosphere, first raise the temperature from room temperature to 300°C for 55 minutes and keep it for 60 minutes, then raise the temperature to 800°C at a heating rate of 5°C / min. Keep for 120min, then naturally cool to room temperature to obtain material B2;

[0033] Step S3: Transfer the material B2 to a 20 wt% hydrofluoric acid solution, soak it for 24 hours, wash it with high-purity water until neutral, and then dry it in an oven at 80°C for 12 hours to obtain the target product C2.

Embodiment 3

[0035] Step S1: Dissolve 5g of melamine and 5mL of formaldehyde in 50mL of deionized water, place in a water bath at 60°C and stir for 30min to mix evenly, then add 1g of SiO 2 , 0.7g iron acetylacetonate and 2mL glacial acetic acid, continue to stir at this temperature for 1h, then stir overnight at room temperature, obtain material A3 by centrifugation and drying:

[0036] Step S2: Transfer the material A3 to a nickel boat and place it in a tube furnace. In an inert gas atmosphere, first raise the temperature from room temperature to 300°C for 55 minutes and keep it for 60 minutes, then raise the temperature to 800°C at a heating rate of 5°C / min. Keep for 120min, then naturally cool to room temperature to obtain material B3;

[0037] Step S3: Transfer the material B3 into a 20 wt% hydrofluoric acid solution, soak it for 24 hours, wash it with high-purity water until neutral, and then dry it in an oven at 80°C for 12 hours to obtain the target product C3.

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Abstract

The invention discloses a preparation method of a Fe / Fe3C nanoparticle-loaded porous nitrogen-doped carbon-based oxygen reduction catalyst, which comprises the following steps of by using SiO2 as a hard template, carrying out polymerization reaction on hydroxymethylated melamine and ferric acetylacetonate to prepare the novel Fe / Fe3C nanoparticle-loaded porous nitrogen-doped carbon-based oxygen reduction catalyst. The polymer containing iron, nitrogen and carbon is synthesized through polymerization reaction of hydroxymethylated melamine and ferric acetylacetonate, the graphitization degree of carbon can be effectively improved through Fe / Fe3C species formed in the pyrolysis process, the electrical conductivity of the material is enhanced, and then the catalytic activity of the catalytic material is improved. The specific surface area of the Fe / Fe3C nanoparticle-loaded porous nitrogen-doped carbon-based oxygen reduction catalyst prepared by the method is 1084 m<2>g<-1>, the average pore diameter is 7 nm, and the Fe / Fe3C nanoparticle-loaded porous nitrogen-doped carbon-based oxygen reduction catalyst has excellent oxygen reduction performance.

Description

technical field [0001] The invention belongs to the technical field of synthesis of non-noble metal doped carbon-based oxygen reduction catalytic materials, in particular to a Fe / Fe 3 Preparation method of C nanoparticle-supported porous nitrogen-doped carbon-based oxygen reduction catalyst. Background technique [0002] The rapid development of industry has brought great social changes, but also brought a series of problems, such as energy crisis, environmental pollution and so on. Therefore, exploring and developing clean and efficient energy conversion devices and energy storage devices is an inevitable way to solve the above problems. As a new type of energy conversion device, fuel cells are considered to be one of the most promising technologies due to their environmental friendliness, low cost, and high energy conversion efficiency. Oxygen reduction reaction (ORR), as a key reaction in the fuel cell cathode, plays an important role in the conversion of chemical energ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/90B82Y30/00B82Y40/00
CPCH01M4/9083H01M4/9075H01M4/9041H01M4/90B82Y30/00B82Y40/00Y02E60/50
Inventor 高书燕张风仙莫振坤刘灿豫王雯辉王坤刘洋
Owner HENAN NORMAL UNIV
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