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Synthesis and Characterization of Carbon/Nitrogen/Iron Based Nanoparticles by Laser Pyrolysis as Non-Noble Metal Electrocatalysts for Oxygen Reduction

CEA, IRAMIS, UMR NIMBE 3685, F-91191 Gif Sur Yvette, France
CEA-Saclay DRF/IRAMIS//SPEC/LNO, 91191 Gif sur Yvette, France
UVSQ, CNRS, UMR 8180, ILV, F-78035 Versailles, France
Author to whom correspondence should be addressed.
Received: 23 May 2018 / Revised: 11 July 2018 / Accepted: 16 July 2018 / Published: 30 July 2018
(This article belongs to the Special Issue Carbon-Based Catalyst)
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This paper reports original results on the synthesis of Carbon/Nitrogen/Iron-based Oxygen Reduction Reaction (ORR) electrocatalysts by CO2 laser pyrolysis. Precursors consisted of two different liquid mixtures containing FeOOH nanoparticles or iron III acetylacetonate as iron precursors, being fed to the reactor as an aerosol of liquid droplets. Carbon and nitrogen were brought by pyridine or a mixture of pyridine and ethanol depending on the iron precursor involved. The use of ammonia as laser energy transfer agent also provided a potential nitrogen source. For each liquid precursor mixture, several syntheses were conducted through the step-by-step modification of NH3 flow volume fraction, so-called R parameter. We found that various feature such as the synthesis production yield or the nanomaterial iron and carbon content, showed identical trends as a function of R for each liquid precursor mixture. The obtained nanomaterials consisted in composite nanostructures in which iron based nanoparticles are, to varying degrees, encapsulated by a presumably nitrogen doped carbon shell. Combining X-ray diffraction and Mossbauer spectroscopy with acid leaching treatment and extensive XPS surface analysis allowed the difficult question of the nature of the formed iron phases to be addressed. Besides metal and carbide iron phases, data suggest the formation of iron nitride phase at high R values. Interestingly, electrochemical measurements reveal that the higher R the higher the onset potential for the ORR, what suggests the need of iron-nitride phase existence for the formation of active sites towards the ORR. View Full-Text
Keywords: laser pyrolysis; non-noble metal electrocatalyst; oxygen reduction laser pyrolysis; non-noble metal electrocatalyst; oxygen reduction

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This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited (CC BY 4.0).

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Perez, H.; Jorda, V.; Bonville, P.; Vigneron, J.; Frégnaux, M.; Etcheberry, A.; Quinsac, A.; Habert, A.; Leconte, Y. Synthesis and Characterization of Carbon/Nitrogen/Iron Based Nanoparticles by Laser Pyrolysis as Non-Noble Metal Electrocatalysts for Oxygen Reduction. C 2018, 4, 43.

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