Iron oxide nanoparticles: the Influence of synthesis method and size on composition and magnetic properties

Iron oxide nanoparticles with mean diameter ranging from 7 to 20 nm were synthesized using two routes: the precipitation method in controlled atmosphere and a reduction–precipitation method under air, in some cases followed by a hydrothermal treatment. The smallest nanoparticles were obtained by the reduction–precipitation method.In order to establish the composition of the iron oxide nanoparticles and its relation with size, the morphological, structural and magnetic properties of the prepared samples were investigated using X-ray diffraction, transmission electron microscopy, Mössbauer spectroscopy and SQUID magnetometry. The results allow to conclude that the nanoparticles can be essentially described as Fe3−xO4, x decreasing with the particle size increase. The composition and magnetic behavior of the synthesized iron oxide nanoparticles are directly related with their size. The overall results are compatible with a core@shell structure model, where a magnetite core is surrounded by an oxidized magnetite layer (labeled as maghemite), the magnetite core dimension depending on the average particle size.

TEM images and Mössbauer spectroscopy spectra of Fe3−xO4 samples with different sizes.Figure optionsDownload as PowerPoint slideHighlights
► Fe3−xO4 nanoparticles with a mean size between 7 and 20 nm were synthesized.
► The smallest nanoparticles were obtained by a reduction precipitation method, under air.
► The increase of particles size was succeeded using a hydrothermal treatment at 150 °C.
► The magnetic properties of the nanoparticles are directly related with their size.