Nanosized TiO2 particles have been prepared by top down approach using mechanical milling with high energy planetary ball mill at 250rpm for different extents of time (5, 10, 20, 30 and 40h). Electroless (EL) Ni–P–TiO2 nanocomposite coatings were developed using alkaline bath containing milled TiO2 nanoparticles (4g/l). The results show that, the morphology of TiO2 particles milled for 40h exhibit irregular shape with a particle diameter in the range of 33–45nm. Wear studies of the coatings with 30μm thickness were investigated using 1, 1.5 and 2N loads with 0.1 and 0.2m/s rotation speeds. The Ni–P–TiO2 nanocomposite coatings exhibit the enhanced hardness and wear resistance as compared to that of Ni–P alloy coatings. Also the composite after heat treatment at 400°C for 1h in argon atmosphere showed improved hardness (1010VHN) and wear resistance (1.5e-06mm3/Nm).