Green and low temperature synthesis of nanocrystalline transition metal ferrites by simple wet chemistry routes

Abstract

Crystalline and nanostructured cobalt (CoFe2O4), nickel (NiFe2O4), zinc (ZnFe2O4) and manganese (MnFe2O4) spinel ferrites are synthesized with high yields, crystallinity and purity through an easy, quick, reproducible and low-temperature hydrothermal assisted route starting from an aqueous suspension of coprecipitated metal oxalates. The use of water as a reaction medium is a further advantage of the chosen protocol. Additionally, the zinc spinel is also prepared through an alternative route combining coprecipitation of oxalates from an aqueous solution with thermal decomposition under reflux conditions. The nanocrystalline powders are obtained as a pure crystalline phase already at the extremely low temperature of 75 °C and no further thermal treatment is needed. The structure and microstructure of the prepared materials is investigated by means of X-ray powder diffraction (XRPD), while X-ray photoelectron spectroscopy (XPS) and inductively coupled plasma-atomic emission spectroscopy (ICP-AES) analyses are used to gain information about the surface and bulk composition of the samples, respectively, confirming the expected stoichiometry. To investigate the effect of the synthesis protocol on the morphology of the obtained ferrites, transmission electron microscopy (TEM) observations are performed on selected samples. The magnetic properties of the cobalt and manganese spinels are also investigated using a superconducting quantum device magnetometer (SQUID) revealing hard and soft ferrimagnetic behavior, respectively.