Abstract: This study determined the optimal concentration of titanium diboride (TiB₂) particles for the development of in situ titanium-titanium boride (Ti-TiB) metal matrix composites (MMCs) prepared by a conventional powder metallurgy route to be used for industrial applications. The effect of concentration of TiB₂ particles was studied by reinforcing TiB₂ powder in different mass fractions (2wt%, 5wt%, 10wt%, and 20wt%) into pure Ti powder during the fabrication process. The MMCs were sintered at high temperatures under vacuum. The transmission electron microscopy (TEM) results revealed the formation of needle-shaped TiB whiskers, indicating that in situ reaction occurred during vacuum sintering of the powder compacts. All the composite samples had a high sintered density, and the hardness of the composites increased with an increase in the mass fraction of reinforcement. Mechanical and tribological properties such as flexural strength, impact, and wear properties were determined and found to be dependent on the mass fraction of the reinforcement. However, the mechanism for the in situ reaction needs further investigation by high-energy in situ X-ray diffraction techniques.