Zirconium aluminium oxynitride multiphase composite film is deposited on zirconium substrate using energetic nitrogen ions delivered from dense plasma Focus device. X-ray diffractometer (XRD) results show that five Focus shots are sufficient to initiate the nucleation of ZrN and Al2O3 whereas 10 Focus shots are sufficient to initiate the nucleation of AlN. XRD results reveal that crystal growth of nitrides/oxides increases by increasing Focus shots (up to 30 Focus shots) and resputtering of the previously deposited film is taken place by further increase in Focus shots (40 Focus shots). Scanning electron microscopic (SEM) results indicate the uniform distribution of spherical grains (similar to 35 nm). A smoother surface is observed for 20 Focus shots at 08 angular position. SEM results also show a net-type microstructure (thread like features) of the sample treated for 30 Focus shots whereas rough surface morphology is observed for 40 Focus shots. Energy dispersive spectroscopic profiles show the distribution of different elements present in the deposited composite films. A typical microhardness value of the deposited composite films is 5255 +/- 10 MPa for 10 grams imposed load which is 3.3 times than the microhardness values of unexposed sample. The microhardness values of the exposed samples increases with increasing Focus shots (up to 30 Focus shots) and decreases for 40 Focus shots treatment due to resputtering of the previously deposited composite film. The microhardness values of the composite films decreases by increasing the sample's angular position. (C) 2009 Elsevier B. V. All rights reserved.