Non-stoichiometric NbxNy coatings, produced in a reactive sputtering process, were analyzed on the basis of their chemical composition (specifically, nitrogen concentration) and its relationship with electrical conductivity. The chemical composition and bonding configuration were examined using X-ray photoelectron spectroscopy (XPS), revealing Nb–N bonds. The stoichiometry variation dependence on the N2 flow was also analyzed, using Auger electron spectroscopy (AES). Without exposing the samples to air, a normal behavior was observed; meaning that the nitrogen concentration in the coatings increased, with an increase in N2 flow. The electrical properties were evaluated and their relationship with nitrogen content in the films was analyzed. The highest conductivity value for all studied samples was observed for the sub-stoichiometric film, NbN0.32, which also exhibited a positive Hall coefficient. It indicated that the conduction was mainly dominated by hole-type carriers. High conductivity at lower nitrogen content was attributed to the fact that, at a low concentration of nitrogen, the effect of impurities, acting as dispersion points for electrons, was lower, increasing the relaxation time. As the main conclusion, the Ar/N2 flow ratio strongly influenced the coatings of stoichiometry and then, this stoichiometry affected, to a great extent, the electrical conduction and the Hall coefficient of the coatings.
In this work, thin films of TaN were synthesized on 304 steel substrates using the reactive DC sputtering technique from a tantalum target in a nitrogen/argon atmosphere. All synthesis parameters such as gas ratio, pressure, gas flow, and substrate distance, among others, were fixed except the applied power of the source for different deposited coatings. The effect of the target power on the formation of the resulting phases and the microstructural and morphological characteristics was studied using XRD and AFM techniques, respectively, in order to understand the growth mechanisms. Phase, line profile, texture, and residual stress analysis were carried out from the X-ray diffraction patterns obtained. Atomic force microscopy analysis allowed us to obtain values for surface grain size and roughness which were related to growth mechanisms in accordance with XRD results. Results obtained showed a strong correlation between the growth energy with the crystallinity of the samples and the formation of the possible phases since the increase in the growth power caused the samples to evolve from an amorphous structure to a cubic monocrystalline structure. For all produced samples, the δ-TaN phase was observed despite the low N2 content used in the process (since for low N2 content it was expected to be possible to obtain films with α-Ta or hexagonal ε-TaN crystalline structure). In order to determine the corrosion resistance of the coatings, electrochemical impedance spectroscopy and polarization resistance were employed in the Tafel region. The results obtained through this evaluation showed a direct relationship between the power used and the improvement of the properties against corrosion for specific grain size values.
Cr, Nb, Cr/Nb, CrNx, NbNx, CrNbN, and (CrN/NbN)n structures were produced on Si and glass substrates, using the d.c. magnetron sputtering technique. Compositional analysis, based on binding energies of Cr, Nb, and N, was carried out by means of X‐ray photoelectron spectroscopy (XPS). Through Auger electron spectroscopy (AES), depth profiles were obtained, allowing to demonstrate the multilayers production. Surface morphological characteristics, as roughness and grain size, were evaluated by atomic force microscopy (AFM), revealing very smooth surfaces, that is a consequence of the deposition parameters used in the synthetization experiments. Finally, for different configurations, conductivity measurements were carried out, revealing the influence of nitrogen content and temperature on electron transport. It was found that substoichiometric nitrides (CrN0.35 and NbN0.12) exhibited the highest conductivity, because the nitrogen atoms act as donor of electrons.
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