Electron diffraction X-ray (EDX) microanalysis and micro-Raman spectroscopy were used to study the annealed semi-conductor surfaces. EDX images showed evidences of two types of regions on the annealed GaAs and GaSb surfaces. Micro-Raman results displayed good proof of two different regions into the surface of both semiconductors, since the spectra of one region showed considerable differences to the spectra of the other. The most notable difference is the transverse optical (TO) activation and the decrease of intensity of other Raman lines in the spectra of very small regions. This work calls attention to the sensibility of micro-Raman experiments to short-length defects, which cannot be detected by EDX analysis. (C) 2002 Elsevier Science B.V. All rights reserved.