Structural and magnetic properties of sonoelectrocrystallized magnetite nanoparticles

Abstract

The effect of ultrasound power on the morphology, structure and magnetic properties of magnetite nanoparticles synthesized from iron electrodes by the electro-oxidation method was investigated. Samples made in aqueous solution in the absence or presence of an organic stabilizer (thiourea, tetramethylammonium chloride, sodium butanoate or β-cyclodextrine) were characterized by x-ray diffraction, transmission and scanning electron microscopy, magnetometry and Mössbauer spectrometry. The iron is almost all in the form of 20–85 nm particles of slightly nonstoichiometric Fe3−δO4, with δ ≈ 0.10. Formation of a paramagnetic secondary phase in the presence of sodium butanoate or β-cyclodextrine is supressed by ultrasound. Specific magnetization of the magnetite nanoparticles ranges from 19 to 90 A m2 kg−1 at room temperature, and it increases with particle size in each series. The particles show no sign of superparamagnetism, and the anhysteretic and practically temperature-independent magnetization curves are associated with a stable magnetic vortex state throughout the size range. The spin structure of the particles and the use of magnetization measurements to detect magnetite in unknown mixtures are discussed.