Nanocomposites comprising bismuth vanadate and molybdenum sulfide were prepared using a hydrothermal route. The concentration of molybdenum sulfide was varied in bismuth vanadate nanostructures to improve their energy storage performance. The prepared samples were used to characterize their structural, morphological, textural, and electrochemical properties. X-ray diffractometry results showed that the crystal structure and phase of bismuth vanadate and molybdenum sulfide nanostructures were monoclinic BiVO4 and rhombohedral MoS2, respectively. The bending and stretching vibrations of the fundamental units of the prepared materials were studied using Raman spectroscopy. Morphological analysis revealed the presence of nanosphere-like structures in the pristine sample, and MoS2 addition led to the formation of additional voids between the nanospheres. BET studies were used to quantify the specific surface areas of the prepared materials. The maximum specific surface area of 8.6 m2 g–1 was obtained for the composite consisting of bismuth vanadate and 3 wt% molybdenum sulfide, while pristine bismuth vanadate nanostructures are endowed with 5.7m2g–1. In addition, the distribution of various pore sizes on the surface of the prepared materials was analysed using the BJH method. The pore size decreased by 34.4% for 3 wt% molybdenum sulfide added bismuth vanadate (1.98 nm) nanostructures. However, the pore volume increased to 0.04 cc g–1, which is 3.3 times higher than that of pristine bismuth vanadate (0.012 cc g–1). Furthermore, the electrochemical performance of the prepared electrodes was studied using a three-electrode electrochemical cell in 2 M KOH electrolytes. All studies indicate that the prepared electrodes stored energy through redox reactions, resembling battery type behaviour. The performance of bismuth vanadate was boosted by increasing the concentration of molybdenum sulfide, which increased the diffusion contribution. A maximum specific capacity of 536 C g–1 was estimated at a specific current of 2 A g–1 for the bismuth vanadate electrodes, with the addition of 3 wt% of molybdenum sulfide. It is nearly 2.45 times higher compared to pristine bismuth vanadate electrodes (219 C g–1). Thus, all analyses suggest that the bismuth vanadate electrodes with 3 wt% molybdenum sulfide are the suitable material for energy storage applications.