. In this work, we present a simple method to fabricate high quality Ni/NiO multilayers with the use of a single magnetron sputtering head. Namely, at the end of the deposition of each single Ni layer, air is let to flow into the vacuum chamber through a leak valve. Then, a very thin NiO layer (~ 1nm) is formed by natural oxidation. The process is reproducible and the result is the formation of a multilayer with excellent layering. Magnetization hysteresis loops recorded at 5 K and room temperature reveal a tendency for perpendicular magnetic anisotropy as the thickness of the individual Ni layers decreases. It is shown that the Ni/NiO interface has sizeable positive surface/interface anisotropy, i.e. it favors the development of perpendicular magnetic anisotropy. This is rather unusual for a Ni-based multilayered system and may render Ni/NiO multilayers useful for magneto-optical recording applications.