Composite NiP-TiO2 layers were prepared by simultaneous electroless deposition of Ni-P and TiO2 on steel substrate, from a solution in which TiO2 particles were kept in suspension by stirring. Deposits were characterized for its Structure, morphology and hardness. It was found that the chemical composition of Ni-P matrix has been influenced by the incorporation of TiO2 particles. TiO2 particle incorporation increases with increase in their bath concentrations (0.5-2.0g/l). An improvement (up to 20%) in micro-hardness was observed in both as plated and vacuum heat-treated composite coatings compared to Ni-P coatings. Electroless deposited composite coatings exhibit an amorphous structure of the nickel matrix in which crystalline titanium oxide is incorporated. Vacuum heat treatment leads to the formation of a crystalline layer in which the Ni and Ni3P Crystallites appear apart from those of the TiO2 (anatase). Potentiodynamic polarization measurements made on these deposits in 3.5 wt.% sodium chloride solution showed decrease in the corrosion resistance for the as-plated and heat-treated composite coatings. (C) 2009 Elsevier Ltd. All rights reserved.