Аннотация:The main goal of this study is the preparation of single-phase MgFe2O4 and Mg(Fe0.8Ga0.2)2O4 powders using a gel auto-combustion method. X-ray powder diffraction (PXRD), micro-X-ray fluorescencespectrometry (μ-XRF), CHNS elemental analysis, scanning and transmission electron microscopies (SEMand TEM) methods have been used to characterize morphology and chemical composition of the synthesized sample. The cationic distribution in the ferrites has been evaluated from the 57Fe Mössbauer spectroscopy measurements. Mössbauer measurements were used to characterize the paramagnet-ferrimagnet phase transition in MgFe2O4.