In the presented work, the conditions of the high-temperature and mechanochemical method for the synthesis of compound Sm5VO10 and their influence on its physicochemical properties were studied.The following methods were used for the study: X-ray powder diffraction (XRD), differential thermal analysis (DTA), infrared spectroscopy (FTIR), ultraviolet and visible light spectroscopy (UV-VIS-DRS), scanning electron microscopy (SEM-EDX), and laser beam diffraction spectrometry (LDS).Based on the results, it was determined that the compound Sm5VO10 is thermally stable in air atmospheres up to 1475 °C, crystallises in a monoclinic system, and its structure is made up of oxygen VO4 and SmO8 polyhedra.The estimated energy gap value for nanometric, mechanochemically obtained Sm5VO10 was about 3.20 eV, and for the microcrystalline, obtained with the high-temperature method, was about 2.75 eV.The established physicochemical characterisation of Sm5VO10 initially showed that the compound could find potential applications, e.g. as a photocatalyst for water purification or as a component of new optoelectronic materials.