The nano-sized thorium(IV) metavanadate is synthesized by microwave-assisted combustion method and the adsorption capacity for efficient removal of nickel ions from aqueous solution has been investigated. The synthesized thorium metavanadate (adsorbent) is characterized using powder X-ray diffraction, FT-IR & Raman spectroscopy, SEM with energy-dispersive X-ray analysis, TEM, surface area analysis, diffused reflectance spectroscopy, and photoluminescence spectroscopy. The adsorption of nickel ions at equilibrium conditions has been studied using the linear form of Langmuir, Freundlich, and Dubinin-Radushkevich isotherm models. Among these models, Langmuir isotherm shows better efficiency with the correlation coefficient (R-2) value of 0.99. The adsorption kinetics of the system is investigated and is found to follow first-order kinetics.