We present the study of the multilayer germanosilicate (Ge:SiO₂) films which have been grown at room temperature, by magnetron sputtering with Ar as a working gas. Each Ge:SiO₂ (molar ratio: 60:40) layer is separated by a pure SiO₂ layer with equal thickness (7.2 nm). The samples were then annealed for 1h at different temperatures Ta (up to 900 °C) which produces Ge nanoparticles. It is shown that the morphology of such a heterogeneous material can be well interpreted by combining the information obtained from the three techniques: grazing incidence wide/small angle x-ray scattering (GIWAXS/GISAXS) and x-ray reflectivity (XR). The analysis of GIWAXS data revealed that the formation of Ge nanoparticles starts at Ta =600°C and that they have maximum fraction at Ta=750 °C. XR superlattice reflections revealed that the period of the multilayer stack decreases for annealed samples: for Ta=600-750 °C by ~1.6 nm (as a result of Ge crystallisation), and for higher Ta by additional 1 nm (crystallisation + out diffusion of Ge atoms from the sample). 2D GISAXS patterns evidence a high degree of vertical alignment of the nanoparticles along whole multilayer stack for Ta= 600-800 °C. The average size of nanoparticles and their in-layer correlation are obtained using Guinier approximation and the position of diffuse scattering maxima, respectively.

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