Thin film multilayers have been the focus of extensive studies recently due to the interesting properties they exhibit. Since the improvement in properties can be attributed directly to the unique nanoscale microstructures, it is essential to understand the factors affecting the microstructural stability in these nanolayer structures. The intermetallic compound, MoSi2, despite its superior oxidation resistance and high melting point, suffers from inadequate high temperature strength and low temperature ductility, properties which hinder its high temperature structural applications . SiC is a potential second phase reinforcement due to its high temperature strength and thermal compatibility with MoSi2. The addition of SiC in a nanolayered configuration has been shown to exhibit significant increase in hardness after annealing . It has also been shown that when annealed above 900°C, the layers break down and grain growth sets in, with a significant decrease in hardness and. Due to the lack of a thermochemical driving force, the two phases remain separate at all temperatures investigated. In this study, the stability of the MoSi2/SiC nanolayers structure under ion irradiation has been investigated.