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The thermal behavior of Ta/Ge superlattices has been studied using Raman spectroscopy. The high‐frequency Raman spectra, obtained as a function of annealing temperature, reveal no significant change in the superlattice structure up to an anneal temperature of 400 °C. The interlayer diffusion at the Ta/Ge interfaces occurs at 500 °C followed by complete crystallization of the superlattice at 600 °C. Raman scattering from the folded acoustic modes of the superlattices was also employed to study the thermal behavior of superlattices, and the results thus obtained corroborate the above findings.