Antimonide-based superlattices dedicated to the elaboration of opto-electronic devices have been studied by X-ray scattering techniques. In particular, specular and non-specular X-ray reflectometry experiments have been performed on two MBE-samples elaborated with different shutter sequences at the interfaces. The results have shown a limitation of the incorporation of Sb species in the subsequent InAs layer for one of the samples, as expected. Then, a study on a InGaAs-cap layer/(InGaAs/AlAsSb)(N) superlattice grown on a InGaAs/InP buffer layer by both specular X-ray reflectometry and High resolution X-ray diffraction is reported. In particular, the results have revealed the presence of a highly disturbed thin-layer on top of the MOVPE-made GaInAs, whose presence has been explained by In-concentration modification during the desoxidation procedure at the surface of the MOVPE-made GaInAs. Beside the results on the Sb-based heterostructures, the use of X-ray scattering metrology as a routinely working non-destructive testing method has been emphasized. (c) 2006 Elsevier B.V. All rights reserved.