Ni O x films were deposited with radio frequency (rf) magnetron sputtering at various sputtering powers (25–300W) and deposition temperatures (room temperature to 200°C) using NiO target and pure O2 as a sputtering gas. Crystallinity, bonding state (Ni+3 and Ni+2), work function, and the resistivity of the film were measured and the performance of the pentacene thin film transistor (TFT) with the NiOx film as a source/drain (S/D) electrode was evaluated. The film properties such as roughness, work function, crystallinity, and bonding state of Ni and O were similar at each sputtering power, and the NiOx film was deposited at around 150W and room temperature showed lower resistivity of 1.34×104μΩcm, lower surface roughness of 0.206nm, and higher work function of 5.2eV. With the increase in the deposition temperature, the ratio of Ni2+ ions to Ni3+ ions in the NiOx film was increased, the work function was decreased and the resistivity was increased. A pentacene TFT with NiOx film deposited at 150W and room temperature showed a device performance better than that with gold film, with mobility of 0.178cm2∕Vs, threshold voltage of 0.34V, and on/off ratio of 5.0×105.