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Abstract This study investigates the presence of titanium oxynitride bonds in titanium dioxide (TiO₂) thin films grown by atomic layer deposition (ALD) using tetrakis dimethyl amino titanium (TDMAT) and water at temperatures between 150 and 350 °C and its effect on the films’ optical and electrical properties. Compositional analysis using X‐ray photoelectron spectroscopy (XPS) reveals increased incorporation of oxynitride bonds as the process temperature increases. Furthermore, depth profile data demonstrates an increase in the abundance of this type of bonding from the surface to the bulk of the films. Ultraviolet‐visible spectroscopy (UV‐vis) measurements correlate increased visible light absorption for the films with elevated oxynitride incorporation. The optical constants (n, k) of the films show a pronounced dependence on the process temperature that is mirrored in the film conductivity. The detection of oxynitride bonding suggests a secondary reaction pathway in this well‐established ALD process chemistry, that may impact film properties. These findings indicate that the choice of process chemistry and conditions can be used to optimize film properties for optoelectronic applications. 

Typical titanium oxide (TiO2) films are transparent in the visible range, allowing for their index of refraction and thickness to be extracted by single-angle spectroscopic ellipsometry (SE) using a Cauchy model. However, TiO2 films grown by atomic layer deposition (ALD) from tetrakis(dimethylamino)titanium (IV) (TDMAT) and H2O at 350 °C absorb in the visible range due to the formation of Ti-O-N/Ti-N bonds. Single-angle SE is inadequate for extracting the optical constants of these films, as there are more unknowns (n, k, d) than measurable parameters (ψ, Δ). To overcome this limitation, we combined SE with transmission (T) measurements, a method known as SE + T. In the process, we developed an approach to prevent backside deposition on quartz substrates during ALD deposition. When applying a B-spline model to SE + T data, the film thicknesses on the quartz substrates closely matched those on companion Si samples measured via standard lithography. The resulting optical constants indicate a reduced refractive index, n, and increased extinction coefficient, k, when compared to purer TiO2 thin films deposited via a physical vapor deposition (PVD) method, reflecting the influence of nitrogen incorporation on the optical properties. 

Nonlinear refractive index, n2 , values as high as 1±.1x10 -9 cm 2 /W were measured in atomic layer deposition (ALD) grown TiO 2 nanoscale films, using femtosecond thermally managed Z-scan. The several order of magnitude increase in n 2 is believed due to the incorporation of nitrogen during growth.