The present study investigated the influence of heptane and tin process control agents on cube milled Ti–6Al–4V + 0.5 Vol% TiC (Ti–6Al–4V–0.5TiC) powder. A smaller particle size and nar‐row particle distribution was observed for Ti–6Al–4V–0.5TiC powder milled with heptane, while the powder milled with tin showed relatively larger particle size and broader particle distribution due to the cold welding of particles. Hcp phase was observed in the Ti–6Al–4V–0.5TiC powder milled with tin. The formation of fcc Ti(C, H)metastable phase with high lattice strain and interstitial content in Ti–6Al–4V–0.5TiC powder milled with heptane, resulted in higher hardness compared to the powder milled with tin.