Shape memory alloys (SMAs) constitute a unique class of materials that undergo a reversible phase transformation allowing the material to display dramatic stress-induced and temperature-induced deformations which are recoverable. Nickel Titanium (NiTi) SMA has be synthesized with refined grain size by a mechanical alloying process. The SMA is produced through a cold rolling fabrication strategy that yields nanocrystalline product structures. By starting with a stacked sandwich array of individual alloy components and subjecting this sample arrangement to repeated rolling and folding, a metal-metal multilayer composite is created. After the layer thickness is reduced to the nanoscale by multiple cold rolling and folding passes, an alloying and intermediate phase formation reaction is initiated. X-ray diffraction profiles confirm that the primary phase present is intermetallic NiTi phase, which is the phase that displays shape memory behavior. The presence of superelastic behavior and the shape memory effect in the product material is established by mechanical testing. At this refined grain size, the hysteresis stress observed is exceptionally small.