Grain size and its distribution in NiTi thin films sputter-deposited on a heated substrate have been investigated using the small angle x-ray scattering technique. The crystalline particles have a small size and are distributed over a small range of sizes for the films grown at substrate temperatures 370 and 420℃. The results show that the sizes of crystalline particles are about the same. From the x-ray diffraction profiles, the sizes of crystalline particles obtained were 2.40nm and 2.81nm at substrate temperatures of 350 and 420℃, respectively. The morphology of NiTi thin films deposited at different substrate temperatures has been studied by atomic force microscopy. The root mean square roughness calculated for the film deposited at ambient temperature and 420℃ are 1.42 and 2.75nm, respectively.