Ordinary attritor milling of elemental metallic powders under atmospheric condition was utilized to prepare desirable amount of powders for thermal spraying. The effect of different BPR (Ball to Powder weight Ratio) has been investigated in terms of nitridation during milling. To investigate the effect of heat treatment on the formation of dispersed phases, heat treatment to the powder was performed as well. Titanium aluminide coatings with carbonitride dispersed phases were successfully fabricated by low pressure plasma spraying. The hardness and specific wear of the coatings prepared by the powders with different milling conditions was measured so as to investigate the effect of the content of dispersed titanium based carbonitride phases. Experimental results show that the formation of dispersed carbonitride phases depends strongly on milling condition, irrespective of heat treated powders or thermal sprayed coatings, and directly affects the mechanical properties of the coatings. Compared with the phase composition of heated powders and corresponding thermal sprayed coatings, it seems that the temperature of processing the MA powders is also a decisive factor on the phase formation, especially carbonitride phases and oxide phase.