Nanocrystalline Ti0.7Cr0.3C powders were synthesized by mechanical alloying (MA) at room temperature from an elemental mixture of Ti, Cr, and C powders. The samples were investigated using X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy (SEM) with energy-dispersive X-ray spectrometry (EDX). The novelty of our study is to advance our knowledge of the effect of milling time on the evolution of microstructural and morphological changes in the Ti0.7Cr0.3C powders. The XRD results revealed that nanostructured (Ti, Cr)C carbide with an average crystallite size of 11 nm was obtained after 20 h of MA. The SEM results showed that during MA, the morphology process implies repeated cold welding, fracturing, and re-welding of powder particles. TEM investigation revealed that the particles of TiCrC powder ranged in size from 50 to 250 nm.