TiSiN films grown by chemical vapor deposition were characterized to evaluate the properties relevant to the application as a diffusion barrier in Cu-based interconnects. The films were grown using TiI4 + SiI4 + NH3 + H2 chemistry at substrate temperature, 370°C, and SiI4 - to-TiI4 precursor flow rate ratio of 30. The combined results from x-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) revealed that the bulk of Ti32Si21N42 films were predominantly consisted of a mixture of cubic TiN and amorphous SiNx phases. The specific electrical resistivity of the films was about 2000 μΩcm which is a few times higher than that of sputtered TiSiN films having similar composition and thicknesses. The 40 nm-thick barrier appeared to be thermally stable against Cu diffusion at the annealing temperatures up to 550°C. Breakdown of this diffusion barrier occurred at 600°C and was accompanied by the formation of Cu3Si protrusions at the TiSiN/Si interface.