Comparison of different methodologies for obtaining nickel nanoferrites

Nickel nanoferrites were obtained by means of four different synthetic wet-routes: co-precipitation (CP), sonochemistry (SC), sonoelectrochemistry (SE) and electrochemistry (E). The influence of the synthesis method on the structural and magnetic properties of nickel ferrite nanoparticles is studied. Although similar experimental conditions such as temperature, pH and time of synthesis were used, a strong dependence of composition and microstructure on the synthesis procedure is found, as electron microscopy, X-ray diffraction and Mössbauer spectroscopy studies reveal. Whereas by means of the CP and SC methods particles of a small size around 5–10 nm, respectively, and composed by different phases are obtained, the electrochemical routes (E and SE) allow obtaining monodisperse nanoparticles, with sizes ranging from 30 to 40 nm, and very close to stoichiometry. Magnetic characterization evidences a superparamagnetic behavior for samples obtained by CP and SC methods, whereas the electrochemical route leads to ferromagnetic ferrite nanoparticles. - Highlights: • Electrochemical synthesis produces pure NiFe2O4 nanonoparticles with 40 nm particle size. • Coprecipitation and sonochemistry techniques generate NiFe2O4 nanoparticles with impurities. • Nanoparticles obtained by coprecipitation and sonochemistry are superparamagnetic. • Electrochemical and sonoelectrochemical methods produce ferromagnetic nanoparticles