The Co-Ni-MoxOy powders were obtained electrochemically at a constant current density from ammonia electrolyte. Ni and Co were anomalously deposited, inducing Mo deposition, which cannot be deposited separately from aqueous solutions. The obtained Co-Ni-MoxOy powders were investigated by energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), and scanning electon microscope (SEM) methods. Based on the obtained experimental results, it was concluded that the particle size of deposited powders is influenced by the chemical composition of the electrolyte and current density imposed. XRD results suggested that obtained powders were of amorphous structure, although a Co3Mo compound can be formed if certain experimental conditions are applied.