Ni-P-TiO 2 nanocomposite coatings were electrodeposited on copper substrates and influence of TiO 2 nanoparticles concentration on the phase structure, morphology, chemical composition, microhardness, and corrosion behaviour of the coatings was investigated. Results demonstrate that Ni 3 Ti intermetallics form and grow during the electrodeposition of the coatings. This study is the first to report the formation of the intermetallics in the case of electrodeposited Ni-P alloy matrix composite coatings. Moreover, the formation mechanism of the intermetallics is discussed in detail. The formed intermetallics dispersed uniformly throughout the microstructure of the nanocomposite coatings, thereby playing a critical role in improving the mechanical and corrosion-related properties of the coatings. Ni-P-10 g•L −1 TiO 2 nanocomposite coating possessing the highest amount of Ni 3 Ti intermetallic associated with the lowest P content, thereby showing the superior microhardness and corrosion resistance. All in all, the volume fraction of Ni 3 Ti intermetallics is the dominant factor altering the various properties of the coatings.