One-step room temperature synthesis of very small γ-Fe2O3 nanoparticles

•One-step synthesis of 3 nm maghemite nanoparticles is reported.•Maghemite nanoparticles can be synthesized from a ferric solution.•γ-Fe2O3 NPs can be obtained if the precursor has Fe(III) in tetrahedral interstices.•HR-TEM, Mössbauer, XAFS and magnetometry analysis proved the maghemite existence

Very small maghemite nanoparticles (∼3 nm) are obtained through a one-step synthesis at room temperature. The fast neutralization reaction of a ferric solution in a basic medium produces an intermediate phase, presumably two-line ferrihydrite, which in oxidizing conditions is transformed to maghemite nanoparticles. The synthesis of maghemite, as final product of the reaction, was characterized by High-Resolution Transmission Electron Microscopy (HR-TEM), X-ray Absorption Fine Structure (XAFS), Mössbauer spectroscopy, and magnetometry. The XAFS technique allowed the analysis of the crystallographic variations into maghemite nanoparticles as a result of modification in its surface/volume ratio. Mössbauer spectroscopy at low temperature (4.2 K) confirms the presence of Fe(III) in tetrahedral and octahedral interstices, in the stoichiometry corresponding to maghemite. The specific magnetization, M vs H (3 K and 300 K, up to 7 T) and temperature dependence of the magnetization (50 Oe by ZFC mode, 2 K ≤ T ≤ 300 K) indicate that maghemite nanoparticles of 3 nm are in superparamagnetic state with a blocking temperature close to 36 K

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