Non-stoichiometric Ni1-xO thin films were prepared on glass substrate by direct current reactive magnetron sputtering in a large range of oxygen partial pressure (0 ≤ pO2 ≤ 1 Pa). The dependence of the deposited film structure and properties on oxygen stoichiometry were systematically analyzed by X-ray diffraction, X-ray reflectivity, X-ray photoemission spectroscopy, Raman spectroscopy, atomic force microscopy, UV–vis measurements and electrical transport properties measurements.
The deposition rates, surface morphology and opto-electrical properties are very sensitive to the oxygen partial pressure lower than 0.05 Pa due to the presence of metallic nickel cluster phase determined by X-ray diffraction, X-ray reflectivity and XPS spectroscopy. Presence of nanocrystallized NiO phase was highlighted even for pO2 = 0 Pa. For pO2 > 0.05 Pa, only the NiO phase was detected.
Progressive appearance of Ni3+ species is characterized by a fine increase of the lattice parameter and (111) preferred orientation determined by grazing angle X-ray diffraction, fine increase of the X-ray reflectivity critical angle, displacement of the Ni 2p3/2 signal towards lower energy, significant increase of the electrical conductivity and decrease of the total transmittance. Quantification of Ni3+ by XPS method is discussed. We also showed that the use of Raman spectroscopy was relevant for demonstrating the presence of Ni3+ in the Ni1-xO thin films.
Wang, M., Thimont, Y., Presmanes, L., Diao, X. and Barnabé, A., 2017. The effect of the oxygen ratio control of DC reactive magnetron sputtering on as-deposited non stoichiometric NiO thin films. Applied Surface Science, 419, pp.795-801.
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