The paper proposes a new approach to Schiff-base ligand assisted sonochemical synthesis of iron vanadate. In this disquisition, we tried to comparing various factors and reaction condition on morphology, size and uniformity of as-obtained samples. Some parameters including Schiff-base capping agent (Bis(acetylacetone) ethylenediamine=H2acacen), electrolyte (NH4F), solvent and reaction time were investigated to reach optimum condition. XRD, FT-IR, EDS, SEM and TEM were used in order to determine purity and structural morphology of as-synthesized products. Also, we explore the possibility of coupling vanadium pantaoxide into iron vanadate that improves optical properties and photocatalytic activity. With this in mind, FeVO4/V2O5 nanocomposite was prepared via in-situ ultrasound-assisted procedure by using NH4F in one step. Influence of different parameters such as type of dye (Rhodamine B=Rh B, Phenol red=Ph R and Methyl violet=MV) and light source (Ultraviolet and visible) on photocatalytic ability of samples were studied.