Soutenance de thèse : Vivian INÊS DOS SANTOS

Development of Alumina-Toughened Zirconia composites reinforced with carbon nanofibers via Direct Ink Writing

Doctorante : Vivian INÊS DOS SANTOS

Laboratoire INSA : MATEIS

Ecole doctorale : ED34 : Matériaux de Lyon

The growing demand for ceramic materials with increasingly complex shapes for biomedical engineering applications cannot be achieved via traditional ceramic processing techniques. Recently, increasing attention has been drawn to ceramic-based materials produced by the additive manufacturing method of direct ink writing (DIW); still, the current challenge remains the achievement of strong mechanical reliability. Hence, in its first chapter, this thesis examines the overall scenario of the DIW field, analyzing the outcomes of published studies, discussing the most innovative approaches and mechanical and biological improvement strategies. The second chapter provides a comprehensive rheological characterization of pastes encompassing an alumina- toughened zirconia (ATZ) powder, a deflocculant, a binder, deionized water and, in some cases, carbon nanofibers (CNFs). Printability tests were also conducted and the results were compared to established printability criteria/parameters (ф, K and FTI), which were found to be suitable for assessing printability with some limitations. Furthermore, a new criterion based on the recovery rate of the storage modulus was introduced, with the potential to predict printability with a single test. The third and last chapter developed DIW-filaments of the same ATZ composite with and without CNFs with the objective of enhancing mechanical properties by CNF orientation. Nozzle diameters of 200-840 µm were used and optimal debinding and sintering conditions were determined, using both Conventional Sintering (CS) and Spark Plasma Sintering (SPS) methods. Were determined: the fracture stress, fracture strain, Young's modulus and mechanical reliability (Weibull modulus). The addition of the CNFs hindered most of the mechanical properties because of their agglomeration. Printing with smaller nozzles improved the Young’s modulus, with ATZ filaments sintered by CS exhibiting transformation-induced plasticity, while those sintered by SPS didn’t. The mechanical properties obtained were comparable to or higher than those achieved through conventional ceramic processing techniques. Similarly, a good level of mechanical reliability was achieved.