Phase composition and morphology characteristics of ceria-stabilized zirconia powders obtained via sol-gel method with various pH conditions

Purpose: High purity, fine crystalline, degradation-free at low temperature powders have attracted special interest in CAD/CAM prosthetic dentistry full ceramic restorations. This study reports the preparation and characterisation of zirconia-ceria (0.9 ZrO₂ 0.1 CeO₂) powders. Materials were obtained from zirconium-n-alkoxide and cerium nitrate hexahydrate in the pH 2–4 and 8–10. Methods: Zirconia-ceria powders were obtained with the sol-gel method in a humid-free environment. Thermal analysis (TGA/DTA) of the as-prepared materials was made for an assessment of its behaviour at elevated temperatures. Specimens were dried at 80 °C and calcinated in two stages: at 300 °C with soaking time 2.5 h and 850 °C with holding time 2.5 h, in order to evaluate the phase transformations. Thermal analyses of the as-dried powders were made for an assessment of its thermal behaviour during heat treatment up to 1000 °C. By X-ray diffraction (XRD), polymorphs of ZrO₂ were identified. Additionally, scanning electron microscopy (SEM) and laser particle size distribution (PSD) were involved for characterisation of morphology of the powders. Results: A correlation between the pH of the colloidal system and the morphology of the as-obtained powders were found. Based on analysis (SEM, PSD), structures were identified known as soft and hard agglomerates. Conclusions: It can be stated that differences found between powder morphology were dependent on the value pH used, which can be crucial for powder densification during sintering and compacting green bodies which, as a consequence, may be crucial for the lifetime of zirconia prostheses. Correlations between phase composition and pH are difficult to grasp, and require further, more sophisticated, studies.