In this paper we present and discuss the surface properties of GaSb substrates correlated to the cleaning procedure. Different etchants were tested and the resulting surfaces were studied by Auger spectroscopy, then by reflection high‐energy electron diffraction and finally annealed under an Sb4flux in order to get a suitable substrate for molecular‐beam epitaxy. From the comparison of the surface properties we show that one of the tested etchants, which associates HCl, HBr, CH3COOH, and HNO3gives the best results: the etch rate can easily be controlled, the cleaned surfaces are smooth (i.e., free of etch pits) and the surface stoichiometry is the least disturbed by the cleaning procedure.