A nanostructured Ti0.8V0.2C solid solution carbide was successfully synthesized via high-energy mechanical alloying (MA) of elemental Ti, V, and C powders for 20 h in a planetary ball mill under argon atmosphere. Phase evolution and microstructural transformation were tracked using XRD, SEM/EDX, and TEM. Progressive alloying resulted in continuous refinement of the carbide structure, where the crystallite size was reduced to similar to 11-15 nm and the lattice microstrain increased up to 0.93 % after 20 h of MA. TEM observations confirmed the formation of highly dispersed nanocrystalline Ti0.8V0.2C solid-solution carbide particles with sizes of 15-20 nm. This work demonstrates the effectiveness of MA in generating a novel Ti-V-based nanocarbide solid solution and highlights the critical role of milling duration in tailoring structural refinement and defect accumulation at the nanoscale.