Thin-films of Ni and Ti were formed by sputter co-deposition of Ni and Ti onto amorphous SiO2 and single crystal NaCl and Sapphire substrates. Films were characterized as follows: a) The chemical composition of the films was analysed by EDAX b) The gross morphology was examined by Scanning Electron Microscopy. c) The crystal phases were indentified by X-ray diffraction and Electron diffraction. Intermetallic NiTi has been identified in samples annealed in vacuo at 850°C. Annealing at 500°C in vacuum produced chemical separation of the Ni and Ti. This effect may be due to a narrow solidus region for the existence of NiTi and inhomogeneities due to uneven deposition of the Ni and Ti.