Thermal anneal treatments are used to identify the temperature range of the two dominant diffusion mechanisms – bulk and grain boundary. To assess the transition between mechanisms, the low temperature range for bulk diffusion is established utilizing the decay of static concentration waves in composition-modulated nanolaminates. These multilayered structures are synthesized using vapor deposition methods as thermal evaporation and magnetron sputtering. However, at low temperature the kinetics of grain-boundary diffusion are much faster than bulk diffusion. The synthesis of Au-Cu alloys (0-20 wt.% Cu) with grain sizes as small as 5 nm is accomplished using pulsed electro-deposition. Since the nanocrystalline grain structure is thermally unstable, these structures are ideal for measuring the kinetics of grain boundary diffusion as measured by coarsening of grain size with low temperature anneal treatments. A transition in the dominant mechanism for grain growth from grain boundary to bulk diffusion is found with an increase in temperature. The activation energy for bulk diffusion is found to be 1.8 eV·atom-1 whereas that for grain growth at low temperatures is only 0.2 eV·atom-1. The temperature for transitioning from the dominant mechanism of grain boundary to bulk diffusion is found to be 57% of the alloy melt temperature and is dependent on composition.