A hybrid cathodic arc and ion beam sputtering method was employed to synthesize Ti-Si-N films. The influence of negative substrate bias on the structure and mechanical properties was investigated by using XRD, XPS, HRTEM, nanoindentor and so on. With the increasing of negative bias there is a decrease in the TiN crystallite size from 36 nm to 10 nm. Negative substrate bias promoted the conformation of nc-TiN/a-Si3N4 nanocomposite structure with complete phase separation and uniform crystallite size. Superhard TiSiN films with a maximum hardness of 46 GPa were successfully synthesized under 100 V negative bias. Severe oxidation occurred in films deposited under 200 V and 300 V negative substrate bias due to the decreasing of deposition rate, which led to the hardness of films reduced to the value of 26 GPa and 22 GPa respectively. (C) 2012 Elsevier B. V. All rights reserved.