The use of plasma sprayed ceramic coats as thermal barrier coatings (TBCs) for the protection of metallic structures and equipment from severe thermal, abrasive and corrosive conditions has been documented extensively in the last two decades. The state-of-the-art TBCs consist of a double layer coat. a top ceramic layer and an intermediate bond coat (MCrAIY, M=Ni, Co, Fe) deposited on the alloy substrate. Zirconia, both stabilized and partially stabilized with different oxides has been used as the ceramic top coat due to its low thermal conductivity and low thermal expansion coefficient. Studies of the microstructure of the TBCs have shown aspects that can help the understanding of the properties of the coating. The ternary system ZrOz-Y203-TiCz is believed to offer improved properties when it is compared to Zr02-Y203. However, the use of &02-Y203-Ti02 as TBCs, a major part of this work, is not widely reported in the literature. The purpose of this thesis was to study the microstructure of a plasma sprayed ZrOrY203-TiO2 TBC using X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive Spectroscopy (EDS), and Transmission Electron Microscopy (TEM). The evolution of the Zr41_phase distribution in the ceramic coat was followed by XRD after different heat treatments, with the finding that the cooling rate plays a decisive role in the final Zr42 phase composition. SEM studies allowed a description of the lamellae structure of the Zr02-Y203-TiOz coating. The evolution of the morphology, porosity and crack distribution in the coat after different thermal treatments were followed by SEM. Evidence of incipient sintering is observed in Zr02-Y203-Ti02 coats heated at temperatures higher than 1200 °C. This should lead to poor coating performance. EDS analysis revealed an heterogeneous distribution of titanium through the oating. A detailed microstructural characterization of the as-sprayed coating was done using TEM. Microstructural features such as micro-twins, antiphase-boundaries and mottled morphology associated with "non-transformable" tetragonal ZrO2 phase were identified. It is believed that these microstructural elements promote toughening and thermal stress relief mechanisms that provide the coating with the erosion and thermal shock resistance required for a TBC. The presence of TiO2 is linked to a higher proportion of tetragonal ZrO2 in the Zr02-Y203-Ti02 coating, therefore improved properties of the coating are expected. The addition of TiO2 promotes grain growth and decreases the final density in pressed and sintered Zr02-Y203-TiO2 powders. The results obtained are a contribution to the understanding of the microstructure of TBCs and to the sparse knowledge base of the ZrOrY2O3-TiO2 coatings. Further work should be done in the characterization of the ZrO2-Y2O3-Ti42 coatings and the study of its stability under different conditions in order to determine the real potential of this material offers as an alternative to the better known ZrOrY203 TBC.