Multilayered metal films including such couples as Ta-Permalloy (Ni80Fe20) play a key role in magnetic recording sensors, where it is important to preserve the integrity of the thin permalloy layer under thermal conditions during processing and subsequent service. Earlier work1 has indicated a fast grain boundary diffusion of Ta in Ni films at temperatures as low as 250°C. In this paper, we report measurements of the kinetics of this diffusion, in the temperature range 300–400°C. For this work, layered Ni/Ta systems were prepared under controlled conditions, annealed in a helium-flow furnace, and characterized by RBS, AES, XRD and SEM. The possible consequences of diffusion on magnetic performance are also discussed.