The active mass of the plates of aspent car battery with higher wear after an efficient desulfatization can be used as sources of a new electrode. This paper proposes the recycling of spent electrodes from a lead acid battery and the incorporation of NiO or Co3O4contents by the melt-quenching method in order to enrich the electrochemical properties. The analysis of X-ray diffractograms indicates the gradual decrease in the sulfated crystalline phases, respectively, 4PbO·PbSO4and PbO·PbSO4phases, until their disappearance for higher dopant concentrations. Infrared (IR) spectra show a decreasing trend in the intensity of the bands corresponding to the sulfate ions and a conversion of [PbO3] pyramidal units into [PbO4] tetrahedral units by doping with high dopant levels, yielding to the apparition of the PbO2crystalline phase. The observed electron paramagnetic resonance (EPR) spectra confirm three signals located on the gyromagnetic factor,g~2, 2.2 and 8 assigned to the nickel ions in higher oxidation states as well as the metallic nickel nanoparticles. This compositional evolution can be explained by considering a process of the drastic reduction in nickel ions from the superior oxidation states to metallic nickel. The linewidth and the intensity of the resonance lines situated at aboutg~2, 2.17, 4.22 and 7.8 are attributed to the Co+2ions from the EPR data. The best reversibility of the cyclic voltammograms was highlighted for the samples withx= 10 mol% of NiO and 15 mol% of Co3O4, which are recommended as suitable in applications as new electrodes for the lead acid battery.