Heat treatment of evaporated Si in contact with Ag films and Ge in contact with Al films results in the formation of precipitates of the semiconductor in a metal matrix. The structure of these precipitates was studied by transmission electron microscopy and diffraction (TEMD) and MeV4He ion channeling techniques. TEMD studies showed that the semiconductor precipitates were crystalline in nature. Channeling techniques showed that the crystallites did not have a simple orientation relationship with the underlying single‐crystal substrate.