Nanocrystalline 3 mol% yttria-tetragonal zirconia polycrystal (3Y-TZP) ceramic powder containing 5 wt.% Al2O3 with 64 m2/g specific area was synthesized through precipitation method. Different amounts of Co (0–3 mol%) were introduced into synthesized powders, and ceramic materials were obtained by heat treatment in the air for 2 h at 1350–1550 °C. The influence of Co addition on the sintering temperature, phase composition, microstructure, mechanical and biomedical properties of the obtained composite materials, and on the resolution of the digital light processing (DLP) printed and sintered ceramic samples was investigated. The addition of a low amount of Co (0.33 mol%) allows us to decrease the sintering temperature, to improve the mechanical properties of ceramics, to preserve the nanoscale size of grains at 1350–1400 °C. The further increase of Co concentration resulted in the formation of both substitutional and interstitial sites in solid solution and appearance of CoAl2O4 confirmed by UV-visible spectroscopy, which stimulates grain growth. Due to the prevention of enlarging grains and to the formation of the dense microstructure in ceramic based on the tetragonal ZrO2 and Al2O3 with 0.33 mol% Co the bending strength of 720 ± 33 MPa was obtained after sintering at 1400 °C. The obtained materials demonstrated the absence of cytotoxicity and good cytocompatibility. The formation of blue CoAl2O4 allows us to improve the resolution of DLP based stereolithographic printed green bodies and sintered samples of the ceramics based on ZrO2-Al2O3. The developed materials and technology could be the basis for 3D manufacturing of bioceramic implants for medicine.
The use of a nanostructured graphene-zirconia composite will allow the development of new materials with improved performance properties and a high functionality. This work covers a stepwise study related to the creation of a nanostructured composite based on ZrO2 and graphene. A composite was prepared using two suspensions: nano-zirconia obtained by sol-gel synthesis and oxygen-free graphene obtained sonochemically. The morphology of oxygen-free graphene sheets, phase composition and the morphology of a zirconia powder, and the morphology of the synthesized composite were studied. The effect of the graphene sheets on the rheological and sintering properties of a nanostructured zirconia-based composite powder has been studied. It has been found that graphene sheets in a hybrid nanostructure make it difficult to press at the elastic deformation stage, and the composite passes into the plastic region at a lower pressure than a single nano-zirconia. A sintering mechanism was proposed for a composite with a graphene content of 0.635 wt%, in which graphene is an important factor affecting the process mechanism. It has been determined that the activation energy of the composite sintering is more than two times higher than for a single nano-zirconia. Apparently, due to the van der Waals interaction, the graphene sheets partially stabilize the zirconia and prevent the disordering of the surface monolayers of its nanocrystals and premelting prior to the sintering. This leads to an increase in the activation energy of the composite sintering, and its sintering occurs, according to a mixed mechanism, in which the grain boundary diffusion predominates, in contrast to the single nano-zirconia sintering, which occurs through a viscous flow.
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