The current work shows the optimization in the preparation of nanosized titanium carbide (TiC) in-situ through mechanical alloying (MA). Metallic titanium (Ti) powders, along with two carbon sources, carbon nanotubes (CNTs), and stearic acid (SA), were used to reduce the particle size using a high-energy Spex800 mill. The combined use of 2 wt % of these carbon sources and n-heptane as a liquid process control agent (PCA) proved crucial in generating nanoscale powder composites through a simple and scalable synthesis process within a 4-hour timeframe. The use of 20 wt % of both carbon sources was compared to determine the ability of CNTs to form carbides and the decomposition of PCAs during mechanical milling. The result reveals structures like nanoblocks and nanolumps with and important size reduction. The structure and morphology of the composites and starting materials were evaluated through x-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), and transmission electron microscopy (TEM).