There is increasing interest in the epitaxial growth of high quality InSb thin films on GaAs substrates for many device applications such as infrared optoelectronics. The large lattice mismatch (14.6%) between InSb and GaAs has meant that both growth techniques and conditions have a large influence on the interface properties and consequently the film quality. A surface science study, by X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES) together with Nomarski microscopy, on the surface and interface properties of InSb/GaAs by metalorganic chemical vapor deposition is presented. It is found fromthe XPS data that the ambient surface is composed of InSb, In2O3, Sb2O3 and Sb2O5. The interdiffusion phenomena are studied by AES depth profiling; the width of interdiffusion region is determined to be 50±10 nm for all the samples grown at different V/III ratios. This is narrower than the data previously obtained for InSb/GaAs interfaces produced by metalorganic magnetron sputtering. The results also demonstrate that uniform and stoichiometric InSb films have been obtained, and that the reproducibility of the MOCVD technique is excellent.