Porous nickel oxide (NiO) nanoflakes are grown by the chemical bath deposition. The thin films are produced on an ITO/glass substrate and annealed at a variable temperature in a furnace. The structural and optical properties and the surface morphology of the thin films are studied and analyzed. FESEM results display the presence of nanoflakes with the structure of NiO/Ni(OH)2 in thin films that appear to increase in size with the annealing temperature. The sample grown at 300 ∘ C is observed to have the highest surface area dimension. The EDX result reveals that the atomic ratio and weight of the treated sample has a non-stoichiometric value, which results in the-type behavior of the NiO thin film. The result obtained by AFM indicates the highest roughness value (47.9 nm) for a sample grown at 300 ∘ C. The analysis on XRD shows that the NiO nanoflakes possess a cubic structure with the orientation peaks of (111), (200), and (220). This appears with a stronger intensity at 300 ∘ C. Likewise, XRD result approves the absence of the Ni(OH)2 peak at the annealing. For the optical band gap, the UV-Vis measurements give a lower value of 3.80 eV for 300 ∘ C due to the highest crystallinity. The optimum temperature to synthesize high-quality NiO nanoflakes is 300 ∘ C, which can be an important factor for good sensing devices. K e y w o r d s: annealing temperature, nanoflakes, thin film, chemical bath deposition, nickel oxide.