Nickel oxide is a promising material for transparent electronics applications. This semiconductor demonstrates the possibility of modifying its physical properties depending on the method of growth and subsequent processing. Here the effects of the discharge power are reported during reactive dc magnetron sputtering, as well as the modes of subsequent annealing of NiO films, on their structural, electrical, and optical properties. NiO films are annealed at various temperatures both in an oxygen-containing environment and under vacuum conditions. Deposited NiO films have a polycrystalline structure with a preferred orientation (200) for the low discharge power mode and (111) for the high discharge power mode. However, obtained NiO films exhibit crystallinity improvement after annealing. The presence of both Ni2+ and Ni3+ oxidation states in the deposited films is found. In addition, it is shown that the relative carrier concentration (Ni3+/Ni2+ peak area ratio) can be controlled by choosing the NiO film preparation mode. The trend in this ratio corresponds to the trend in film conductivity and the number of free-charge carriers. The deposited films are semitransparent, and the estimated optical bandgap of NiO is in the range from 3.50 to 3.74 eV. © 2024 The Authors. Advanced Materials Interfaces published by Wiley-VCH GmbH.