Ion-beam assisted synthesis and thermal oxidation of TiN thin films combined with in-situ, depth-resolved characterization using MeV ions

We present an in-situ, depth-resolved and non-destructive approach to assess the chemical composition of titanium nitride (TiN) thin films during synthesis and controlled oxidation. Ion beam assisted deposition was used to deposit a TiN sample of approximately 120 nm thickness. The chemical composition was characterized in the deposition environment using non-destructive Rutherford/Elastic Backscattering Spectrometry (RBS/EBS), with a depth resolution of ca. 25 nm. The high sensitivity of the measurements to the non-metallic species was ensured by the use of elastic resonances. Analysis revealed a few percent oxygen incorporated in the films due to residual gases during growth. After deposition, the TiN film was exposed to oxygen at step-wise increasing temperatures, and the composition of the film was analyzed after every annealing step. The measurements provide a direct proof of inward oxidation with associated concentration gradients, starting with oxygen absorption without significant nitrogen release when using moderate annealing temperatures (250–310 °C), where the oxygen content tends to saturation. At 710 °C, above the oxidation onset temperature, atomic composition data indicate N loss parallel to the O uptake. However, ex-situ transmission electron microscopy showed no evidence of any oxide phase, implying that oxidation starts without crystallite formation.