Nanomaterials are of great interest due to their applications in many fields. The structural and efficacy of nano-materials depend strongly on the method applied for their synthesis. In this work, nanosized nickel oxide (NiO) particles were prepared by pulsed laser ablation (PLA) technique in 3% H2O2 aqueous solution The structural and optical properties of the NiO were investigated by X-ray diffractometer (XRD), field emission scanning electron microscope (FE-SEM), energy dispersive X-ray spectroscope (EDX), UV-Vis spectroscopy and Fourier-transform infrared spectroscopy (FT-IR). XRD analysis confirms that the phase is pure nickel oxide with lattice parameter = 0.42033 nm and 8 nm grain size while photoluminescence emission spectrum showed strong peak at 3.62 eV attributed to the band edge transition. FT-IR spectra depicts a strong band at similar to 450 cm(-1) which corresponds to the bending vibration of Ni-O bond. This work demonstrates that PLA is an effective method to control the size, impurity and minimal chemical waste generation which is the major problem with other wet chemical methods. (C) 2012 Elsevier B. V. All rights reserved.