Pulsed laser ablation in liquid (PLAL) has been widely applied for the generation of nanoparticles (NPs). We report on the generation of NiO NPs using a high-power, high-brightness continuous wave (CW) fiber laser source at a wavelength of 1,070 nm. Characterization of such NPs in terms of size distribution, shape, chemical composition, and phase structure was carried out by transmission electron microscopy (TEM), high-resolution TEM equipped with energy-dispersive X-ray (EDX), and X-ray diffraction (XRD). The results revealed the formation of NiO NPs in water with an average size of 12.6 nm. The addition of anionic surfactant sodium dodecyl sulfate (SDS) reduced the size of NiO NPs down to 10.4 nm. The shape of the NPs was also affected by the SDS, showing the change of shapes from spherical domination in water to tetragonal with increased SDS concentrations. Furthermore, the NiO NPs generated in water and SDS solutions were dual phase containing both cubic and rhombohedral structures. It was also found that the NiO NPs were single crystalline in nature irrespective of the size and shape.