An intelligent material Nb-Al, expected to produce intermetallics phase instantaneously to stop crack development upon collision with sub-centimeter sized hypervelocity space debris, is researched. Intermetallics-free Nb-Al powders are produced through mechanical alloying (MA) and densification achieved through spark plasma sintering. Nb-Al powders are mechanically alloyed using planetary ball mill using agate and zirconia pot. Rotation speed and milling time is changed systematically to form intermetallics-free critical MA powder. A state of ultra fine intermetallics-free Nb-Al powder is produced. Intermetallics-free MA powder with fine Nb in Al matrix with most minute average particle size is utilized and sintering was carried out in vacuum with axial pressure increased up to 1.5GPa. The sintered compacts are then subjected to test such as XRD profiling, FE-SEM observation and mechanical properties testing such as hardness, etc.