Mechanosynthesis, structural, thermal and magnetic characteristics of oleic acid coated Fe3O4 nanoparticles

Oleic acid coated iron ferrite-magnetite nanoparticles (Fe3O4) have been synthesized via a new combined route, ceramic method and subsequent wet mechanical milling, starting from a stoichiometric mixture of the easily accessible Fe and Fe2O3 precursors. In the first step, the magnetite has been obtained in well crystallised state by heat treatment of precursor's mixture. In the second step, the as obtained magnetite powder has been wet milled in a high energy planetary ball mill using oleic acid as process control agent. Using the same conditions dry milled magnetite samples have been obtained for comparison. The as obtained powders have been characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FUR), magnetic measurements M = f(H), scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). According to XRD analysis two different processing mechanisms are observed for dry and wet milling modes. The magnetite mean crystallite size is 19 nm according to XRD after 240 min of wet mechanical milling. The High Resolution SEM confirmed that the powder consists in nanoparticles that have particles with the size up to 30 nm. The bond of the oleic acid to the magnetite nanoparticles has been observed by FTIR and DSC investigations. The presence of free and bonded oleic acid is revealed and the free oleic acid can be removed controlled by heat treatment. The magnetisation of the milled samples is lower as compared to the magnetisation of the un-milled sample due to several causes such as disordered structure, finite size effect and powder contamination. A powder contamination with iron occurs during milling and this leads to the formation of a wiistite-FeO phase for the dry milled samples. In the case of the wet milled samples, due to an oleic acid layer the FeO phase formation is prevented. (C) 2016 Elsevier B.V. All rights reserved.