Nitrogen-doped graphitization carbon encapsulation iron nanoparticle preparation method

A graphitized carbon and nanoparticle technology, applied in chemical instruments and methods, nanotechnology, chemical/physical processes, etc., can solve problems such as differences and differences in preparation methods

Active Publication Date: 2015-05-13
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Publicly reported non-noble metal catalysts for oxygen reduction reactions usually contain carbon, nitrogen, and transition metals (iron, cobalt, etc.), but the carbon sources, nitrogen sources, and transition metal compounds used are different, and the preparation methods are also different.

Method used

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  • Nitrogen-doped graphitization carbon encapsulation iron nanoparticle preparation method
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  • Nitrogen-doped graphitization carbon encapsulation iron nanoparticle preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 10g ferric ammonium citrate and 1g dicyandiamide and dissolve them in 150mL water respectively, mix well and remove the solvent at 90°C; put the solid mixture in a quartz boat, then put it into a tube furnace equipped with a quartz tube, At a flow rate of 100mL min -1 Under nitrogen atmosphere, at 5°C min -1 Raise the temperature to 600 °C at a rate of 5 hours, and take it out after cooling to room temperature. The obtained solid was dissolved in 0.1molL -1 HClO 4 The solution is treated under stirring at 80° C. for 24 hours, filtered and washed with water and dried to obtain a nitrogen-doped graphitized carbon-encapsulated iron nanoparticle material.

Embodiment 2

[0030] Weigh 10g of ferric ammonium citrate and 10g of dicyandiamide and dissolve them in 150ml of water respectively, mix well and remove the solvent at 90°C; put the solid mixture in a quartz boat, then put it into a tube furnace equipped with a quartz tube, At a flow rate of 50mL min -1 Under argon atmosphere, at 10°C min -1 Raise the temperature at a rate of 800°C and keep it for 2 hours, and take it out after cooling to room temperature. Dilute the obtained solid in 1molL -1 In the HCl solution, the mixture was treated at 80° C. for 24 hours under stirring, filtered and washed with water and dried to obtain a nitrogen-doped graphitized carbon-encapsulated iron nanoparticle material.

Embodiment 3

[0032] Weigh 1g of ferric ammonium citrate and 20g of dicyandiamide and dissolve them in 300mL of water respectively, mix well and remove the solvent at 90°C; put the solid mixture in a quartz boat, and then put it into a tube furnace equipped with a quartz tube, At a flow rate of 150mL min -1 Under nitrogen atmosphere, at 20°C min -1 The temperature was raised to 1100° C. and kept for 3 hours, then cooled to room temperature and taken out. The obtained solid was dissolved in 0.5molL -1 HNO 3 The solution is treated under stirring at 80° C. for 24 hours, filtered and washed with water and dried to obtain a nitrogen-doped graphitized carbon-encapsulated iron nanoparticle material.

[0033] The relevant parameter of prepared material in the embodiment 1-3 of table 1

[0034]

[0035] In the material of the present invention, the size of iron nanoparticles is between 1-20nm, the iron loading is between 2-20wt%, and the content of doped nitrogen is between 1-10wt%. The mat...

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Abstract

The present invention discloses a nitrogen-doped graphitization carbon encapsulation iron nanoparticle preparation method, which comprises: dissolving ammonium ferric citrate and dicyanodiamide in water, uniformly mixing, heating, removing the solvent to obtain solid powder, placing the solid powder in a quartz boat, placing into a tube type furnace provided with a quartz tube, introducing an inert gas, heating to a temperature of 500-1100 DEG C, maintaining for 0.5-7 h, cooling to a room temperature, treating the obtained solid for 12-36 h in an acid solution at a temperature of less than 100 DEG C, and carrying out filtration, water washing and drying to obtain the target material. According to the present invention, in the material, the size of the iron nanoparticles is 1-20 nm, the iron loading amount is 2-20 wt%, and the nitrogen doping amount is 1-10 wt%; the material has the high electrocatalysis activity when the material is applied for the proton exchange membrane fuel cell cathode oxygen reduction reaction; and the used precursor of the present method is inexpensive, the preparation process is simple, and the large-scale preparation can be achieved.

Description

technical field [0001] The invention relates to a method for preparing nitrogen-doped graphitized carbon-encapsulated iron nanoparticles by using a mixture of ferric ammonium citrate and dicyandiamide as a precursor through heat treatment and acid treatment. Background technique [0002] The proton exchange membrane fuel cell is a power generation device that directly converts the chemical energy of the fuel into electrical energy through an electrochemical reaction without combustion. The cathode oxygen reduction reaction is an important factor affecting the performance of proton exchange membrane fuel cells. Currently widely used platinum-based noble metal catalysts are limited in reserves and expensive, which greatly restricts the application of proton exchange membrane fuel cells. In recent years, seeking cheap catalysts to replace noble metals and improve their electrocatalytic performance has received more and more attention. The reported non-noble metal catalysts fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24H01M4/90B82Y40/00
CPCY02E60/50
Inventor 汪国雄王静谭大力包信和
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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