Magnesium with its mechanical properties and nontoxicity is predetermined as a material for biomedical applications; however, its high reactivity is a limiting factor for its usage. Powder metallurgy is one of the promising methods for the enhancement of material mechanical properties and, due to the introduced plastic deformation, can also have a positive influence on corrosion resistance. Pure magnesium samples were prepared via powder metallurgy. Compacting pressures from 100 MPa to 500 MPa were used for samples’ preparation at room temperature and elevated temperatures. The microstructure of the obtained compacts was analyzed in terms of microscopy. The three-point bendisng test and microhardness testing were adopted to define the compacts’ mechanical properties, discussing the results with respect to fractographic analysis. Electrochemical corrosion properties analyzed with electrochemical impedance spectroscopy carried out in HBSS (Hank’s Balanced Salt Solution) and enriched HBSS were correlated with the metallographic analysis of the corrosion process. Cold compacted materials were very brittle with low strength (up to 50 MPa) and microhardness (up to 50 HV (load: 0.025 kg)) and degraded rapidly in both solutions. Hot pressed materials yielded much higher strength (up to 250 MPa) and microhardness (up to 65 HV (load: 0.025 kg)), and the electrochemical characteristics were significantly better when compared to the cold compacted samples. Temperatures of 300 °C and 400 °C and high compacting pressures from 300 MPa to 500 MPa had a positive influence on material bonding, mechanical and electrochemical properties. A compacting temperature of 500 °C had a detrimental effect on material compaction when using pressure above 200 MPa.
Zirconia ceramics are used in a wide range of applications, including dental restorations, bioimplants, and fuel cells, due to their accessibility, biocompatibility, chemical resistance, and favorable mechanical properties. Following the development of 3D printing technologies, it is possible to rapidly print zirconia-based objects with high precision using stereolithography (SLA) and digital light processing (DLP) techniques. The advantages of these techniques include the ability to print multiple objects simultaneously on the printing platform. To align with the quality standards, it is necessary to focus on optimizing processing factors such as the viscosity of the suspension and particle size, as well as the prevention of particle agglomeration and sedimentation during printing, comprising the choice of a suitable debinding and sintering mode. The presented review provides a detailed overview of the recent trends in preparing routes for zirconium oxide bodies; from preparing the suspension through printing and sintering to characterizing mechanical properties. Additionally, the review offers insight into applications of zirconium-based ceramics.
The stability of ceramic suspensions is a key factor in the preparation and shaping of ceramic bodies. The presented work offers an experimental determination of ceramics suspensions stability using the LUMiSizer analytical centrifuge, focusing on kinetic behaviour using transmission profiles and instability indexes. Multiple ceramic systems comprising corundum, metakaolin, and zirconia suspensions were experimentally examined under varying solid contents, dispersant dosages, and additive concentrations. Results showed that highly loaded corundum suspensions with dispersant (Dolapix CE64) achieved excellent stability, with an instability index below 0.05. Compared to classical sedimentation tests, which are time-consuming and not highly sensitive, LUMiSizer offers a suitable alternative by guaranteeing correct kinetic data and instability indexes indicating suspension behaviour using centrifugal force. Comparisons of the LUMiSizer results and data obtained using the modified Stokes law confirmed increased terminal velocities in experiments with metakaolin suspensions, indicating the sensitivity of the centrifuge to the effect of dispersion medium shape. The influence of porogen (waste coffee grounds) on the stability of corundum suspensions was also investigated, followed by slip casting to create and characterize a ceramic body, confirming the possibility of shaping based on stability results. Furthermore, instability indices are suggested as a rapid, quantitative method for comparing system stability and as an auxiliary criterion to the rheological measurements. Optimal dispersant concentration for zirconia-based photocurable suspensions was identified as 8.5 wt.%, which minimized viscosity and, at the same time, assured maximal kinetic stability. Integrating the LUMiSizer analytical centrifuge with standard methods, including sedimentation tests and rheological measurements, highlights its value as a powerful tool for characterizing and optimizing ceramic suspensions.
10 September 2024 in Journal of Thermal Analysis and Calorimetry
Calcium aluminate phases have a particular effect on the early heat release during setting initiation and have a substantial influence on the further workability of ordinary Portland cement. The nature of the calcium aluminate hydration products and its kinetics strongly depends on sulfate content and humidity. The effect of mineralisers on melt formation and viscosity is well described for calcium silicate systems, but information is still lacking for calcium aluminates. Therefore, the synergistic effect on the crystal structure and hydration mechanism of the tricalcium aluminate phase of the addition of mineralizers, i.e. Li2O, CuO, SO3 to the raw meal is here investigated. Co-doped calcium aluminate structures were formed during high-temperature treatment. Thermal analysis (TG–DTA and heating microscopy) was used to describe the ongoing high-temperature reaction. Resulting phase composition was dependent on the concentration of the mineralizer. While phase pure system was prepared with low mineralizer concentrations, with increasing mineralizer content the secondary phases were formed. Raman spectroscopy and XPS analysis were used to investigate the cation substitution and to help describe the cations bonding in co-doped calcium aluminate system. Prepared powders have been hydrated in a controlled manner at different temperatures (288, 298, 308 K). The resulting calorimetric data have been used to investigate the hydration kinetics and determine the rate constant of hydration reaction. First-order reaction (FOR) model was here applied for the activation energy and frequency factor calculations. The metastable and stable calcium aluminate hydrates were formed according to initial phase composition. In phase pure systems with low S content, the formation of stable and metastable hydrates was depended on the reaction temperature. Conversely, in systems with secondary phases and higher S content, the hydration mechanism resembled that which appears in calcium sulfoaluminates.