Due to their high capacitance, stability, and conductivity, binary transition metal oxides, such as iron vanadate, have the potential to be ideal electrode materials for supercapacitors. The effect of surfactants such as Polyethylene glycol (PEG), cetyltrimethylammonium bromide (CTAB), and thioglycolic acid (TGA) on the formation and properties (structural, morphological, optical and vibrational) of iron vanadate nanoparticles has been investigated using various analytical techniques. The results show that the surfactants significantly influence the morphology of the prepared FeVO4 nanoparticles. The nanoparticles prepared using TGA show a nano-mat like structure with the smallest particle size, and they were subjected to Cyclic Voltammetry analysis, showing a specific capacitance of 48 Fg−1 and demonstrating potential to be used for supercapacitors.