The direct observation of nickel (Ni) impurities in lightly doped ferromagnetic polycrystalline (ZnNi)O was discussed. Polycrystalline ZnNiO powder samples were synthesized by an auto-combustion method from zinc nitrate, nickel nitrate, and glycine. The particle morphology and selected area electron diffraction (SAED) patterns were obtained using a JEOL model 1200 EX transmission electron microscope. The results show that the weight percentages of Ni metal impurity calculated from the magnetization data are almost comparable to that obtained from XRD data, indicating that ferromagnetic contributions are mainly coming from the Ni secondary phase present in the samples.