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Solid oxide fuel cells (SOFC) operating in the temperature range between 800–1000 °C are devices converting directly chemical energy into electrical energy. The SOFC electrolyte layer typically consisting of yttria-stabilized zirconia (YSZ) was prepared using atmospheric plasma spraying technology. Plasma spraying is a cost-effective technique for the production of functional layers in SOFCs and allows the optimization of the layers' porosity that affects the fuel cell performance (e.g., life-time). Raman spectroscopy is a powerful tool for the investigation of structural features, for example, crystallinity, molecular orientation, and phase composition, especially of inorganic thin films. In order to get further information concerning the thin-film properties of plasma-sprayed zirconia-based electrolytes X-ray diffraction (XRD) as well as scanning electron microscopy (SEM) were applied. In this study we show that depending on the preparation conditions the crystal growth and the density of the plasma-sprayed thin films can be influenced significantly. Therefore Raman spectra as well as XRD and SEM pictures show subtle differences concerning the crystallinity of various samples. Raman Spectroscopic Investigation of Plasma-Sprayed Zirconia-Based Electrolytes