The present study describes the synthesis of CeO₂-CNiO nanoflakes (CeNiO-NFs) via solution process in a very short time span and it was utilized for to control the growth against liver and breast cancer cells. The processed nanocomposites were characterized with several instruments such as of their physicochemical characteristics such as XRD, FT-IR, TGA/DTG/DSC, DLS, BET, SEM-EDX, TEM and UV-visible spectrophotometer respectively. The acquired results are in full justification with the physical data and it suggests that the formed CeO₂-CNiO nanocomposite is in nanoflakes shaped (~20-C25 nm). Moreover, anticancer activity of CeNiO-NFs was investigated through MTT and NRU assays for liver (HepG2) and breast (MCF7) cancer cells. The results demonstrated that it exhibited dose-dependent cytotoxic effects in the range of 1-C100 μg/mL and revealed a reduction in their cell viability in response from low and high concentration of CeNiO-NFs.