© 2022, King Fahd University of Petroleum & Minerals.Electrochemical deposition of Ni metal matrix composite coatings is widely used in various applications to improve corrosion resistance and hardness of the materials. In this study, the Ni-Cu and Ni-Cu/CeO2 metal matrix coatings were fabricated via electrodeposition on SS 304 substrates. The cyclic voltammetry measurements suggest that the addition of CeO2 particles into the electrolyte shifted hydrogen evolution reaction to more negative potentials and slightly accelerated the deposition of Ni ions. The compositional analyses also suggested a higher Ni fraction for the deposit with CeO2 containing electrolyte. The structural characterization through XRD measurements showed the presence of Ni-Cu solid solutions for all coatings and the presence of CeO2 for the ceramic reinforced layer. The crystal size of the Ni-Cu solid solutions ranged between 10 and 20 nm. It was observed that the morphology of the coatings was cauliflower and the size of the cauliflowers changed to a bigger size and turned into compacted layer with the addition of CeO2 into electrolyte. Deposits without CeO2 showed smaller and more localized separated cauliflowers, whereas coatings with CeO2 showed denser layer. The hardness of the samples increased from 317 ± 19 to 475 ± 18 HV and the corrosion current density decreased from 48.8 to 36.5 µA/cm2 with the addition of CeO2 suggesting an improved performance for Ni-Cu/CeO2 metal matrix composite coating. The Nyquist and Bode plots supported the findings in the potentiodynamic polarization tests.