A structural, magnetic and colloidal stability study of uncoated and silica coated iron oxide samples prepared in two different surfactants

Abstract

The discovery of new magnetic materials of interest in the biomedicine field is a relevant topic in current research. For years, our research group has been investigating the obtaining and study of nanostructured magnetic samples that behave superparamagnetically to enable their transport in living organisms. We present here a study that summarizes the structural characteristics, magnetic behavior and stability of two Fe3O4 samples synthesized by coprecipitation that were dispersed using two different surfactants (oleylamine, OL, and oleic acid, OA), and two others prepared from the previous ones by reaction with tetraethyl orthosilicate (TEOS). The relationships between the surfactant used in the synthesis, the presence of a certain maghemite (γ-Fe2O3) content, the influence of silica shell thickness and magnetic behaviour of all samples were systematically studied by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), Mössbauer spectroscopy and H vs. M loops. Rietveld refinements of the XRD profiles confirmed a partial oxidation of the non-silica-coated samples and FTIR spectra of the uncoated samples showed a very strong broad metal-oxygen band and additional sets of bands from the different organic chains of the two surfactants. Individual particles with a mean diameter of 7 and 9 nm were distinguished in TEM images of uncoated magnetic samples. Mössbauer data indicated the presence of non-stoichiometric magnetite in all samples, in agreement with XRD refinements. Magnetic measurements confirmed the superparamagnetic behavior of all the samples. Highest negative zeta potential values are found for the silica covered samples in both acidic and basic medium, being Fe3O4-AO@SiO2 the best suited for the purposes of its dispersibility in future applications. Low polydispersity index (PDI) values confirmed the best stability and dispersibility of all samples investigated in tetrahydrofuran (THF).