MgFe2O4 powders with nanosize (30-100 nm) were synthesized by the solgel auto combustion method. These powders were calcined at various temperatures (300°C, 400°C, 500°C, 600°C, 700°C, 800°C). An increase in particle size was observed as a function of calcination temperature. The appearance of α-Fe2O3 in samples calcined at intermediate temperatures was studied by XRD, Raman spectra and was confirmed using magnetization data. © 2013 American Institute of Physics.