Multilayer films, consisting of alternating layers of crystalline Ni and Ti, have been prepared by RF sputter deposition over a range of modulation wavelengths corresponding to an overall composition of Ni50Ti50. These films have been characterized by xray diffraction and Rutherford backscattering measurements. The solid-state transformation by interdiffusional mixing of the individual layers has been directly studied by differential scanning calorimetry and correlated with structural measurements. These measurements indicate that the solid-state reaction of Ni and Ti multilayers proceeds through the formation of a metastable solid solution of Ti in Ni followed by the formation of intermetallic equilibrium compounds. No direct calorimetric or structural evidence for the formation of an amorphous Ni-Ti phase has been found in these samples.