X-ray reflectivity, diffraction and grazing incidence small angle X-ray scattering as complementary methods in the microstructural study of sol–gel zirconia thin films

X-ray reflectometry, X-ray diffraction and grazing incidence small angle X-ray scattering have been complementary used to fully characterize zirconia (ZrO2) thin films obtained by the sol–gel route. The films were synthesized on various sapphire (Al2O3), silicon (Si) and glass mirrorpolished wafers by a dip-coating process in a zirconia precursor sol. Versus the synthesis parameters as alkoxide sol concentration, withdrawal speed and annealing temperature, the microstructure of the layer is managed and its different microstructural parameters such as thickness, mass density, crystalline phase, grain size and spatial arrangement have been determined. The as prepared layers are amorphous. During a thermal treatment at low temperature (