Density, thickness and composition measurements of TiO2SiO2 thin films by coupling X-ray reflectometry, ellipsometry and electron probe microanalysis-X

Mixed TiO₂SiO₂ thin films were deposited by aerosol atmospheric CVD method by using di-acetoxi di-butoxi silane (DADBS) and Ti tetra-butoxide as precursors. By varying the deposition temperatures between 470 and 600 °C and the ratios between the Si and Ti precursors (Si/Ti) from 2 up to 16, films with different compositions and thicknesses were deposited. The coupled analysis of the results of different characterisation methods was used in order to determine the variation of the composition, the thickness and the density of the films. First EPMA measurements were performed at different acceleration voltages with a Cameca SX50 system. By analysing, with specific software, the evolution of the intensity ratio I_x/I_std versus the voltage, the composition and the mass thickness (product of density by the thickness) were determined. In order to measure independently the density, X-ray reflectometry experiments were performed. By analysing the value of the critical angle and the Kiessig fringes, the density and the thickness of the layers were determined. The refractive index and the thickness of the films were also measured by ellipsometry. By assuming a linear interpolation between the index value of the pure SiO₂ and TiO₂ films, the film composition was deduced from the refractive index value. XPS measurements were also performed in order to obtain an independent value of the composition. A good agreement between the ways to measure the density is obtained.