ABSTRACTWe have succeeded in synthesizing orthorhombic Ga(1−x)Fe(1+x)O3 (−0.05 x0.5), hexagonal GayFe(2−y)O3 (0y1.8) and cubic Ga(1+z)Fe(2−z)O4 (−0.1z0.8) nanograins of gallium ferrites using conventional precursors and an organic environment of Pechini scenario under atmospheric-pressure conditions (SG method). Phase composition and homogeneity were analyzed using X-ray diffraction. Small angle neutron scattering disclosed ellipsoidal particle shapes of gallium iron oxides (GFO) crystallizing in orthorhombic (o-GFO) and hexagonal (h-GFO) symmetry and parallelepiped shapes of Ga(1+y)Fe(2−y)O4 (c-GFO) grains. Despite local agglomeration among the magnetic grains, the scanning electron microscopy and transmission electron microscopy images point to faced-elliptical shapes. The Mössbauer spectroscopy with magnetization measurements was carried out in the temperature range of 5–295 K. The analysis of gallium ferrites magnetism demonstrates that iron atoms locate with various probabilities in crystallographic positions and the spontaneous magnetization preserves up to room temperature (RT).