In aiming at an electronic superlattice, epitaxial structures consisting of alternating layers of GaAs and GaAlAs have been grown by molecular‐beam evaporation. The technique of He‐ion backscattering provides a unique method for the direct and non‐destructive profiling of these structures for superlattice layers of a few hundred angstroms if detailed account is made of the backscattering process. The results of Raman spectroscopy and scanning electron microscopy are shown also to furnish complementary information on compositions and thicknesses, respectively. The three techniques give similar results.