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Genesis of supported carbon-coated Co nanoparticles with controlled magnetic properties, prepared by decomposition of chelate complexes

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Abstract

Following procedures formerly developed for the preparation of supported heterogeneous catalysts, carbon-coated cobalt nanoparticles dispersed on porous alumina have been prepared by impregnation of γ-Al2O3 with (NH4)2[Co(EDTA)] and thermal decomposition in inert atmosphere. Below 350 °C, Co(II) ions are complexed in a hexa-coordinated way by the EDTA ligand. The thermal treatment at 400–900 °C leads to the EDTA ligand decomposition and recovering of the support porosity, initially clogged by the impregnated salt. According to X-ray absorption spectroscopy, and due to in situ redox reactions between the organic ligand and Co(II), both oxidic and metallic cobalt phases are formed. Characterisation by transmission electron microscopy, X-ray diffraction and magnetic measurements reveals that an increase in the treatment temperature leads to an increase of the degree of cobalt reduction as well as to a growth of the cobalt metal particles. As a consequence, the samples prepared at 400–700 °C exhibit superparamagnetism and a saturation magnetisation of 1.7–6.5 emu g−1 at room temperature, whilst the sample prepared at 900 °C has a weak coercivity (0.1 kOe) and a saturation magnetisation of 12 emu g−1. Metal particles are homogeneously dispersed on the support and appear to be protected by carbon; its elimination by a heating in H2 at 400 °C is demonstrated to cause sintering of the metal particles. The route investigated here can be of interest for obtaining porous magnetic adsorbents or carriers with high magnetic moments and low coercivities, in which the magnetic nanoparticles are protected from chemical aggression and sintering by their coating.

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Acknowledgements

The authors thank Dr. Françoise Villain (Laboratoire de Chimie Inorganique et Matériaux Moléculaires, UMR 7071 CNRS, UPMC) for her assistance in recording the XAS spectra, and the French Ministry of National Education and Research for financial support through a grant to KT.

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  1. Laboratoire de Réactivité de Surface (UMR 7197, CNRS), UPMC (Université Pierre et Marie Curie), 4 Place Jussieu, 75252, Paris Cedex 5, France

    Konstantin Tarasov, Patricia Beaunier, Michel Che & Eric Marceau

  2. CNRS, 4 Place Jussieu, 75252, Paris Cedex 5, France

    Konstantin Tarasov, Patricia Beaunier, Michel Che, Eric Marceau & Yanling Li

  3. Institut Parisien de Chimie Moléculaire (IPCM, UMR 7201, CNRS), UPMC (Université Pierre et Marie Curie), 4 Place Jussieu, 75252, Paris Cedex 5, France

    Yanling Li

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  1. Konstantin Tarasov
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Correspondence to Eric Marceau.

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Tarasov, K., Beaunier, P., Che, M. et al. Genesis of supported carbon-coated Co nanoparticles with controlled magnetic properties, prepared by decomposition of chelate complexes. J Nanopart Res 13, 1873–1887 (2011). https://doi.org/10.1007/s11051-010-9938-x

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