The coated system, i.e., nickel basic carbonateshell/copper oxalatecore, were synthesized by heating dispersions, containing various amounts of the cores (copper oxalate particles), urea, and nickel sulfate for different intervals of time at 85 °C. These uniformly coated particles were obtained under narrow set of the experimental conditions. On heat treatment, the shell and core materials transformed independently into their respective oxides and ended up with coated particles composed of nickel oxideshell/copper oxidecore. The above‐mentioned systems of particles were characterized by scanning electron microscopy (SEM), x‐ray diffractometry (XRD), Fourier transform infrared spectrometry (FTIR), and thermogravimetric/differential thermal analysis (TG/DTA).