Microstructural evolution of Au/TiO₂ nanocomposite films: The influence of Au concentration and thermal annealing

Nanocomposite thin films consisting of a dielectric matrix, such as titanium oxide (TiO₂), with embedded gold (Au) nanoparticles were prepared and will be analysed and discussed in detail in the present work. The evolution of morphological and structural features was studied for a wide range of Au concentrations and for annealing treatments in air, for temperatures ranging from 200 to 800 °C. Major findings revealed that for low Au atomic concentrations (at.%), there are only traces of clustering, and just for relatively high annealing temperatures, T ≥ 500 °C. Furthermore, the number of Au nanoparticles is extremely low, even for the highest annealing temperature, T = 800 °C. It is noteworthy that the TiO₂ matrix also crystallizes in the anatase phase for annealing temperatures above 300 °C. For intermediate Au contents (5 at.% ≤ C_Au ≤ 15 at.%), the formation of gold nanoclusters was much more evident, beginning at lower annealing temperatures (T ≥ 200 °C) with sizes ranging from 2 to 25 nm as the temperature increased. A change in the matrix crystallization from anatase to rutile was also observed in this intermediate range of compositions. For the highest Au concentrations (> 20 at.%), the films tended to form relatively larger clusters, with sizes above 20 nm (for T ≥ 400 °C). It is demonstrated that the structural and morphological characteristics of the films are strongly affected by the annealing temperature, as well as by the particular amounts, size and distribution of the Au nanoparticles dispersed in the TiO₂ matrix. - Highlights: • Au:TiO₂ films were produced by magnetron sputtering and post-deposition annealing. • The Au concentration in the films increases with the Au pellet area. • Annealing induced microstructural changes in the films. • The nanoparticle size evolution with temperature depends on the Au concentration