Oxygen out-diffusion in thin CuO films (300 nm thick) deposited on Si (100) substrates has been studied by conventional Rutherford backscattering spectrometry (RBS), 3.045 MeV 16O(α, α)16O resonance, X-ray photoelectron spectroscopy (XPS) depth profiling, and X-ray diffractometry (XRD). Oxygen depletion proceeds progressively inward from the surface inducing a transformation from the initial CuO into Cu2O at temperatures in the range of 450 to 750°C during vacuum annealing. Using the oxygen resonance technique, the oxygen depth profiles for the above given transformation were obtained and they are compared to results obtained by XPS depth profiling.