Ge-rich ZrO2 films, fabricated by confocal RF magnetron sputtering of pure Ge and ZrO2 targets in Ar plasma, were studied by multi-angle laser ellipsometry, Raman scattering, Auger electron spectroscopy, Fourier transform infrared spectroscopy, and X-ray diffraction for varied deposition conditions and annealing treatments. It was found that as-deposited films are homogeneous for all Ge contents, thermal treatment stimulated a phase separation and a formation of crystalline Ge and ZrO2. The “start point” of this process is in the range of 640–700 °C depending on the Ge content. The higher the Ge content, the lower is the temperature necessary for phase separation, nucleation of Ge nanoclusters, and crystallization. Along with this, the crystallization temperature of the tetragonal ZrO2 exceeds that of the Ge phase, which results in the formation of Ge crystallites in an amorphous ZrO2 matrix. The mechanism of phase separation is discussed in detail.

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The change of optical and structural properties of Ge nanoclusters in ZrO 2 matrix have been investigated by spectroscopic ellipsometry versus annealing temperatures. Radio-frequency top-down magnetron sputtering approach was used to produce the samples of different types, i.e. single-layers of pure Ge, pure ZrO 2 and Ge-rich-ZrO 2 as well as multi-layers stacked of 40 periods of 5-nm-Ge-rich-ZrO 2 layers alternated by 5-nm-ZrO 2 ones. Germanium nanoclusters in ZrO 2 host were formed by rapid-thermal annealing at 600-800 • C during 30 s in nitrogen atmosphere. Reference optical properties for pure ZrO 2 and pure Ge have been extracted using single-layer samples. Asdeposited multi-layer structures can be perfectly modeled using the effective medium theory. However, annealed multi-layers demonstrated a significant diffusion of elements that was confirmed by medium energy ion scattering measurements. This fact prevents fitting of such annealed structure either by homogeneous or by periodic multi-layer models.

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