Abstract: | This paper aims to characterise the systems NiFe2O4/SiO2 and CoFe2O4/SiO2 prepared by the sol-gel method. After heat treatment, the various samples have been studied by means of X-ray diffraction, Mössbauer spectroscopy, magnetic measurements and transmission electron microscopy (HR TEM).X-ray diffraction and Mössbauer spectra confirmed the presence of the spinel phase. HR TEM observations revealed the nanocrystals with the size in the range of 2–25 nm. Magnetic measurements showed a superparamagnetic behaviour of the samples heated at lower temperature (800°C) and ferrimagnetic character for the samples heated at higher temperature (900, 1000°C).The final phase composition of the heated samples depends on the preparation conditions. The samples, treated up to 300°C in vacuum and then subsequently heated at 800°C or 900°C, do not contain hematite (the most stable phase at higher temperatures). On the contrary, the samples heated at 1000°C or 1250°C display certain content of hematite. |