TiB 2/ Si 3 N 4 nano multilayers have been synthesized under different deposition parameters related to substrate by ion beam assisted deposition (IBAD). XRD, Nano indenter, profiler, and multi-functional tester for material surface properties were used to characterize the microstructure and mechanical properties of the multilayers. The results indicated a well-defined composition modulation and layer structure of the multilayers. To the multilayers with constant modulation ratio of 15.4:1 and modulation period of 11.8 nm, the multilayer deposited on Al 2 O 3(111) substrate with 38 nm-thick Ti buffer layer at deposition temperature of 225°C revealed the highest hardness (37.4 GPa) and elastic modulus. This hardest multilayer also showed the improved residual stress, friction coefficient, and fracture resistance.