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Influence of synthesis method on structural and magnetic properties of cobalt ferrite nanoparticles

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Abstract

The Co–ferrite nanoparticles having a relatively uniform size distribution around 8 nm were synthesized by three different methods. A simple co-precipitation from aqueous solutions and a co-precipitation in an environment of microemulsions are low temperature methods (50 °C), whereas a thermal decomposition of organo-metallic complexes was performed at elevated temperature of 290 °C. The X-ray diffractometry (XRD) showed spinel structure, and the high-resolution transmission electron microscopy (HRTEM) a good crystallinity of all the nanoparticles. Energy-dispersive X-ray spectroscopy (EDS) showed the composition close to stoichiometric (~CoFe2O4) for both co-precipitated nanoparticles, whereas the nanoparticles prepared by the thermal decomposition were Co-deficient (~Co0.6Fe2.4O4). The X-ray absorption near-edge structure (XANES) analysis showed Co valence of 2+ in all the samples, Fe valence 3+ in both co-precipitated samples, but average Fe valence of 2.7+ in the sample synthesized by thermal decomposition. The variations in cation distribution within the spinel lattice were observed by structural refinement of X-ray absorption fine structure (EXAFS). Like the bulk CoFe2O4, the nanoparticles synthesized at elevated temperature using thermal decomposition displayed inverse spinel structure with the Co ions occupying predominantly octahedral lattice sites, whereas co-precipitated samples showed considerable proportion of cobalt ions occupying tetrahedral sites (nearly 1/3 for the nanoparticles synthesized by co-precipitation from aqueous solutions and almost 1/4 for the nanoparticles synthesized in microemulsions). Magnetic measurements performed at room temperature and at 10 K were in good agreement with the nanoparticles’ composition and the cation distribution in their structure. The presented study clearly shows that the distribution of the cations within the spinel lattice of the ferrite nanoparticles, and consequently their magnetic properties are strongly affected by the synthesis method used.

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Acknowledgments

This work was supported by the Slovenian Research Agency, the Ministry of Higher Education, Science and Technology of the Republic of Slovenia within the National Research Program, and by DESY and the European Community under Contract RII3-CT-2004-506008 (IA-SFS). Provision of synchrotron radiation facilities by HASYLAB is acknowledged. The authors would also like to thank Daša Lesjak for help with the synthesis of the nanoparticles, E. Welter of HASYLAB for expert advice on beamline operation and Paul McGuiness for performing VSM measurements.

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Authors and Affiliations

  1. “Jozef Stefan” Institute, Ljubljana, Slovenia

    Sašo Gyergyek, Darko Makovec, Alojz Kodre, Iztok Arčon & Miha Drofenik

  2. Faculty of Mathematics and Physics, University of Ljubljana, Ljubljana, Slovenia

    Alojz Kodre

  3. University of Nova Gorica, Nova Gorica, Slovenia

    Iztok Arčon

  4. Institute of Mathematics, Physics and Mechanics, Ljubljana, Slovenia

    Marko Jagodič

  5. Faculty of Chemistry and Chemical Engineering, University of Maribor, Maribor, Slovenia

    Miha Drofenik

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  1. Sašo Gyergyek
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  2. Darko Makovec
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  3. Alojz Kodre
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Correspondence to Sašo Gyergyek.

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Gyergyek, S., Makovec, D., Kodre, A. et al. Influence of synthesis method on structural and magnetic properties of cobalt ferrite nanoparticles. J Nanopart Res 12, 1263–1273 (2010). https://doi.org/10.1007/s11051-009-9833-5

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  • DOI: https://doi.org/10.1007/s11051-009-9833-5

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