High energy ball milling (HEBM) had been carried out to produce submicron size titanium aluminide intermetallics (TiAl) using elemental powders of Ti and Al alongwith Ni-P coated graphite. 1% graphite powders was added to stoichiometric composition of Ti48Al and ball milling was conducted for different milling time at varying rpm. The effect of milling time and rpm on particle size has been studied. The prepared samples have been characterized using X-ray diffraction, differential scanning calorimetry (DSC) and scaning elecron microscopy (SEM). Grain size as low as 500 nm could be achieved. Formation of Ti3Al, TiAl and carbon containing intermetallic compounds had been confirmed through X-ray diffraction. Milling time and rpm of mill is found to be important factors which control the final particle size.