Nano-multilayers represent a new class of engineering materials that are made up of alternating nanometer scale layers of two different components. In the present work a titanium (Ti) monolayer was combined with titanium diboride (TiB2) to form a Ti/TiB2 nano-multilayer. Designed experimental parameters enabled an evaluation of the effects of direct current bias voltage (Ub) and bilayer thickness (A) during multilayer deposition on the mechanical properties of reactively sputtered Ti/TiB2 multilayer films. Their nanostructures and mechanical properties were characterized and analyzed using X-ray photoelectron spectroscopy (XPS), low-angle and high-angle X-ray diffraction (XRD), plan-view and cross-sectional high-resolution transmission electron microscopy (HRTEM), and microindentation measurements. Under the optimal bias voltage of U-b=-60 V, it was found that Lambda (varied from 1.1 to 9.8 nm) was the most important factor which dominated the nanostructure and hardness. The hardness values obtained varied from 12 GPa for Ti and 15 GPa for TiB2 monolayers, up to 33 GPa for the hardest Ti/TiB2 multilayer at Lambda = 1.9 nm. The observed hardness enhancement correlated to the layer thickness, followed a relation similar to the Hall-Petch strengthening dependence, with a generalized power of similar to 0.6. In addition, the structural barriers between two materials (hcp Ti/amorphous TiB2) and stress relaxation at interfaces within multilayer films resulted in a reduction of crack propagation and high-hardness. (C) 2007 Elsevier B.V. All rights reserved.