Polycrystalline CdTeCdS heterojunction solar cells are a possible candidate for the low cost, high efficiency conversion of solar energy. The formation of an intermediate CdS x Te 1− x layer during a high temperature annealing stage is believed to increase optical absorption and decrease cell efficiency. S diffusion in single crystal CdTe has been investigated by NRA using the 32S (d,p o) 33S nuclear reaction, at a deuteron energy of 2 MeV. Details of the NRA depth profiling procedure are given, which was found to be relatively straightforward and suitable for use on a small Van de Graaff accelerator. The resulting diffusion parameters are compared to those obtained by SIMS using a Cs + primary ion beam, examining negative secondary ions. The diffusion coefficients were found to be 1.1 × 10 −15cm 2 s −1 at 450°C and ∼8 × 10 −15cm −1 s at 550°C. S diffusion in thin films was also investigated by 2 MeV 4He + RBS on annealed polycrystalline CdSCdTe multilayers.