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Nitrogen-doped graphene-iron-based nanoparticle composite catalyst and preparation method thereof

A nitrogen-doped graphene and nanoparticle technology is applied in the field of electrochemical catalysis to achieve the effects of good cycle stability, excellent methanol tolerance, and high oxygen reduction catalytic activity

Active Publication Date: 2015-12-23
TSINGHUA UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a nitrogen-doped graphene-iron-based nanoparticle composite catalyst and its preparation method for the problem that the performance of the Fe-N-C catalyst still exists and needs to be further improved.

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  • Nitrogen-doped graphene-iron-based nanoparticle composite catalyst and preparation method thereof
  • Nitrogen-doped graphene-iron-based nanoparticle composite catalyst and preparation method thereof

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Embodiment 1

[0027] Step 1: Weigh 80 mg of graphene oxide (Zhongke Times Nano, Chengdu Organic Chemical Co., Ltd.), ultrasonically disperse it in 400 mL of deionized water, and prepare a graphene oxide aqueous solution with a concentration of 0.2 mg / mL. The above graphene oxide aqueous solution was placed in a 1000 mL three-necked flask, 100 μL of hydrazine hydrate solution (80% by mass fraction) was added, and reacted in an oil bath at 95° C. for 1 hour (full magnetic stirring). After the solution was cooled, it was filtered to remove large pieces of reduced graphene oxide to obtain a black water dispersion of reduced graphene oxide (concentration was about 0.15 mg / mL).

[0028] Step 2: Weigh 25 mg of ferric chloride hexahydrate, add it to the above-mentioned reduced graphene oxide dispersion, and stir thoroughly for 12 hours to obtain a mixed solution (the mass ratio of iron content to reduced graphene oxide is about 1:12) , The airgel precursor was obtained after freeze-drying at -62°C....

Embodiment 2

[0032] Step 1: Weigh 200 mg of graphene oxide (Zhongke Times Nano, Chengdu Organic Chemical Co., Ltd.), ultrasonically disperse it in 200 mL of deionized water, and prepare a graphene oxide aqueous solution with a concentration of 1 mg / mL. The graphene oxide aqueous solution was placed in a 500 mL three-necked flask, 800 mg of sodium borohydride was added, and after fully magnetically stirred for 3 hours, it was reacted in a 95° C. oil bath for 1 hour (fully magnetically stirred). After the solution is cooled, filter to remove large pieces of reduced graphene oxide; rinse with a large amount of deionized water to remove residual ions. Finally, a black water dispersion of reduced graphene oxide (concentration about 0.5 mg / mL) was obtained.

[0033] Second step: take by weighing 84mg ferric oxalate pentahydrate, join in the above-mentioned reduced graphene oxide dispersion liquid, obtain mixed solution (the mass ratio of iron content and reduced graphene oxide is about 1:5) afte...

Embodiment 3

[0036] Step 1: Weigh 120 mg of graphene oxide (Zhongke Times Nano, Chengdu Organic Chemical Co., Ltd.), ultrasonically disperse it in 400 mL of deionized water, and prepare a graphene oxide aqueous solution with a concentration of 0.3 mg / mL. The above graphene oxide aqueous solution was placed in a 1000 mL three-necked flask, 150 μL of hydrazine hydrate solution (80% by mass fraction) was added, and reacted in an oil bath at 95°C for 1 hour (full magnetic stirring). After the solution was cooled, it was filtered to remove large pieces of reduced graphene oxide to obtain a black water dispersion of reduced graphene oxide (concentration was about 0.25 mg / mL).

[0037]Second step: take by weighing 90mg ferric nitrate nonahydrate, join in the above-mentioned reduced graphene oxide dispersion liquid, obtain mixed solution (the mass ratio of iron content and reduced graphene oxide is about 1:8) after fully stirring 12 hours, in Airgel precursors were obtained after freeze-drying at ...

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Abstract

The present invention relates to a nitrogen-doped graphene-iron-based nanoparticle composite catalyst and a preparation method thereof, wherein the catalyst is a complex of nitrogen-doped graphene and iron-based nanoparticles (including metal iron and iron nitride). The main preparation process comprises: carrying out a reaction of a graphene oxide aqueous solution and a reducing agent (hydrazine hydrate or sodium borohydride) for 1 h under an oil bath to obtain reduced graphene oxide; mixing the reduced graphene oxide aqueous solution and an iron salt, completely stirring, and carrying out freezing drying to obtain a reduced graphene oxide-iron salt aerogel precursor; and carrying out a high temperature heat treatment under a mixed atmosphere of ammonia gas and an inert gas to obtain the nitrogen-doped graphene and iron-based nanoparticle complex. Compared with the commercial platinum-carbon catalyst, the composite non-precious metal catalyst of the present invention has advantages of simple preparation process, low cost, high oxygen reduction catalysis activity, good methanol tolerance and the like, and can be used for fuel cells, lithium-air batteries and other oxygen reduction catalysis reaction systems.

Description

technical field [0001] The invention belongs to the field of electrochemical catalysis, and relates to a composite catalyst, in particular to a graphene-based non-noble metal composite catalyst for oxygen reduction reaction and a preparation method thereof. Background technique [0002] Today, with the increasing consumption of fossil fuel resources and increasingly serious environmental problems, the development of clean and efficient new energy technologies has become an urgent need. Among them, low-temperature fuel cells such as proton exchange membrane fuel cells and direct alcohol fuel cells, as a clean and pollution-free energy conversion device, have the advantages of high energy density, high energy conversion efficiency, mild working conditions, and fast start-up speed. Widespread concern. So far, the research and development of low-temperature fuel cells have made great progress, but there is still a long way to go before the real large-scale industrial applicatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24H01M4/90
CPCY02E60/50
Inventor 崔肖阳张政军
Owner TSINGHUA UNIV
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