Spinel type structure nickel ferrite (NiFe2O4) and zinc ferrite (ZnFe2O4), as well as nickel zinc ferrite (Ni1-xZnxFe2O4, where x=0,7) compounds were prepared by sol-gel auto-combustion method. Achieved ferrite type compounds were calcinated at different evaluated temperatures from 800oC till 1300oC. Product morphology as result of auto-combustion reaction was investigated by scanning electron microscopy. Structure analysis and crystalline sizes of obtained ferrite compounds were characterized by using x-ray diffraction, but for verifying spinel type solid solution crystallic phases were used infrared spectroscopy. Obtained ferrite sizes were measured by using atom force microscopy. By using corresponding methods, it was demonstrate, that by performing calcination at evaluated temperatures, preferable ferrite compounds in nanoscale dimensions were obtained.