A particulate reinforced NiAl-AlN composite alloy has a NiAl matrix and greater than about 13 volume percent fine particles of AlN within the matrix. The particles preferably have a diameter from about 15 nanometers to about 50 nanometers. The particulate reinforced NiAl-AlN composite alloy may be prepared by cryomilling prealloyed NiAl in liquid nitrogen using grinding media having a diameter of from about 2 mm to about 6 mm at an impeller speed of from about 450 RPM to about 800 RPM. The cryomilling may be done for a duration of from about 4 hours to about 20 hours to obtain a cryomilled powder. The cryomilled powder may be consolidated to form the particulate reinforced NiAl-AlN composite alloy. The particulate reinforced alloy can further include a toughening alloy. The toughening alloy may include NiCrAlY, FeCrAY and FeAl
