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In contrast to complex syntheses for the preparation of colloidal nanocomposites in a core-shell structure proposed in the literature, we present herein a facile colloidal route based on a heterocoagulation process promoted by the electrostatic interaction among ceramic NiO nanoplatelets and metallic Ni nanoparticles (NPs). Before the heterocoagulation process, NiO and Ni were synthetized separately in presence of ultrasound, by chemical precipitation and chemical reduction of the same nickel precursor, respectively. After that, NiO-Ni core-shell nanostructures were prepared forcing the electrostatic interaction among surfaces in aqueous medium. The surface charge balances of both types of particles were tuned effectively by adjusting the pH in a free-additives suspension. For the surface modification of NiO by Ni, the ceramic suspensions maintain a positive zeta potential at pH 9, while the surface of metallic particles is negatively charged. Then the uniform coating of NiO platelets, by the electrostatically induced coagulation with Ni NPs, was favors. The degree of coverage and the formation of NiO-Ni core-shell nanostructures were followed referring the evolution of zeta potential with the geometric calculation in terms of size and morphology of both nanoparticles, and then corroborated by field emission scanning electron microscopy (FESEM).