MgFe2O4-Fe2O3 composites nanostructures were synthesized by different wet chemical methods such as: precipitation, reflux and hydrothermal method. XRD confirmed the formation of composite MgFe2O4-Fe2O3 phase by precipitation, reflux methods and single MgFe2O4 phase by hydrothermal method with well crystalline nature. From FTIR study, the shifting of adsorption bands of metal-oxygen bond corresponding to the vibration of tetrahedral and octahedral complexes of MgFe2O4-Fe2O3 composites was observed than single MgFe2O4 phase. From FESEM images, it is observed that the MgFe2O4-Fe2O3 nanocomposites prepared by precipitation method contains very smooth particles with average diameters around 20-40 nm, the MgFe2O4-Fe2O3 nanocomposites prepared by reflux method contains both uniform microspheres and flower-like hierarchical nanostructures with thickness around 100-200 nm and the MgFe2O4 nanomaterials synthesized by hydrothermal method contains irregular spherical nanoparticles with diameter around 60-100 nm. The prepared nanomaterials were used as photocatalysts to degrade methylene blue dye in aqueous media under solar light irradiation. The MgFe2-O4Fe2O3 nanocomposite prepared by precipitation method was regarded as a superb photocatalyst; 0.1 g of the photocatalyst performed the degradation of 99.9% of methylene blue dye from 100 ml of 10 mg/L solution within 120 mins of irradiation time. (C) 2017 Elsevier B.V. All rights reserved.