Using in situ reflection high energy electron diffraction and x-ray diffraction, the structure and composition of nickel and titanium multilayer films have been studied. The films were evaporated under UHV conditions at rates of.01 to.1 nm/sec. When deposited on an amorphous NiTi film at 70°C, the individual layers of nickel or titanium are polycrystalline and textured with the close-packed planes perpendicular to the growth direction. The interface between the layers is amorphous and about 2 nm thick. X-ray scattering from the crystalline layers indirectly shows the composition of the amorphous interface to be Ni rich.