Current speed sintering and high-speed sintering protocols compromise the translucency but not strength of yttria-stabilized zirconia.

OBJECTIVES: To investigate the impacts of speed and high-speed sintering on the densification, microstructure, phase composition, translucency, and flexural strength of yttria-stabilized zirconia (YSZ). METHODS: A total of 162 disc-shaped specimens (n = 18) were cold-isostatically pressed from 3YSZ (Zpex), 4YSZ (Zpex 4), and 5YSZ (Zpex Smile) powders (Tosoh Corporation) and sintered according to the following protocols: conventional (control, ∼12 h), speed (∼28 min for 3YSZ; ∼60 min for 4YSZ and 5YSZ), and high-speed (∼18 min) sintering. Dimensions of zirconia specimens after sintering and polishing (1-µm diamond grit finish) were Ø13.75 × 1 mm. Density, microstructure, phase content, translucency parameter, and biaxial flexural strength were evaluated using Archimedes', SEM, XRD, spectrophotometric, and piston-on-3-ball methods, respectively. Data were analyzed with either one-way ANOVA and Tukey's test or Kruskal-Wallis with Dunn's test (α = 0.05). RESULTS: For all YSZ compositions, conventional sintering yielded the highest density followed by speed then high-speed sintering. All sintering protocols resulted in similar strength values; however, speed and high-speed sintering protocols afforded significantly lower translucency relative to conventional sintering. XRD analysis revealed similar spectra for YSZs sintered by various protocols. The speed sintered specimens had the smallest grain size whereas the high-speed sintered 5YSZ possessed the largest grain size among all groups. SEM examination of all YSZ compositions revealed that the average pore size was an order of magnitude smaller than the average grain size. SIGNIFICANCE: Speed and high-speed sintering of YSZs yield similar strength but diminished density and translucency relative to their conventionally sintered counterparts.

In vitro comparison of physical characteristics of milled versus printed zirconia discs.

PURPOSE: The purpose of this study was to compare the dimensional accuracy, translucency, and biaxial flexural strength of milled zirconia (MZ) versus 3D-printed zirconia (PZ) discs. MATERIALS & METHODS: A circular disc measuring 14.0 mm in diameter and 1.20 mm in thickness was designed using computer-aided design (CAD) software. The resulting standard tessellation language (STL) file was used both as a control and to fabricate 36 zirconia (3Y-TZP) disc specimens (n = 36): 18 were milled (group MZ) and 18 were 3D-printed (group PZ). The diameter and thickness of each disc were measured using a digital caliper. Translucency was evaluated using a calibrated dental colorimeter. The flexural strength was determined using the piston-on-three-ball biaxial flexure test. All measurements were done by one blinded examiner. The statistical significance level was set to α = 0.05. RESULTS: The MZ discs had significantly more accurate dimensions than the PZ discs in both diameter and thickness when compared to the control CAD software-designed disc. The MZ discs exhibited significantly higher translucency (translucency parameter (TP) = 16.95 ±0.36 vs. 9.24 ±1.98) and biaxial flexural strength (996.16 ±137.37 MPa vs. 845.75 ±266.16 MPa) than the PZ discs. Finally, MZ possessed a significantly higher Weibull modulus relative to PZ. CONCLUSIONS: The results showed that the milled specimens achieved better dimensional accuracy and were more translucent, stronger, and less prone to failure than printed specimens.

Transient thermal stresses developed during speed sintering of 3 mol% yttria-stabilized tetragonal zirconia polycrystals.

OBJECTIVES: To investigate transient thermal stresses that developed in 3Y-TZP green compacts during speed sintering. METHODS: A total of 312 disc-shaped green compacts (Ø17.1 ×1, 1.5, 2, 2.5, 3 mm) were cold-isostatically pressed from 3Y-TZP powder (Zpex, Tosoh Corp.) for speed sintering studies as well as compositional analysis and biaxial flexural strength measurements (both at room temperature and following heating at 90 °C/min to 500 °C). Flexural strength was determined using the piston-on-3-ball method. Phase assemblies were analyzed using the X-ray diffraction method. Effects of heating/cooling rates on transient stresses were investigated by conducting definitive sintering studies to determine the threshold for fracture. Finite element analysis (FEA) was used to validate the experimental findings using measured thermomechanical properties. RESULTS: The bulk and relative density of the green compact were 2.95 ± 0.03 g/cm3 and 48.52% ± 0.45%. The flexural strength was drastically decreased from 10.3 ± 0.4 MPa to 1.09 ± 0.07 MPa following heating at 90 °C/min to 500 °C. The monoclinic and tetragonal contents were 54.9% and 45.1%, respectively. The threshold for fracture was located at 500 °C during the first heating stage with a 90 °C/min heating rate in specimens of 2.5 mm thickness or greater. No fractures occurred in the second heating stage and cooling phase. The FEA estimated that the principal transient tensile stress was ∼1.14 MPa at 500 °C during the heating phase, which exceeded the corresponding flexural strength (1.09 ± 0.07 MPa). SIGNIFICANCE: Advanced FEA methods are an accurate and efficient tool to analyze the history of transient stresses during sintering of ceramic dental restorations.

Survivability and fracture resistance of monolithic and multi-yttria-layered zirconia crowns as a function of yttria content: A mastication simulation study.

OBJECTIVE: To compare four different types of monolithic zirconia crowns in terms of survival rate and fracture resistance after thermocycling and/or thermo-mechanical loading in a chewing simulator. METHODS: Partially stabilized zirconia (PSZ) crowns with fiber-reinforced resin die assemblies (n = 80) were fabricated using: multi-yttria-layered 5Y-PSZ/3Y-PSZ, multi-yttria-layered 5Y-PSZ/4Y-PSZ, monolithic 4Y-PSZ, and monolithic 3Y-PSZ as control (n = 20). Half of the samples in each group were subjected to thermo-mechanical loading under 110 N, 1.4 Hz, 1.2 million cycles with simultaneous thermocycling (10,000 cycles, 5-55°C). The other half were subjected to thermocycling alone. The samples were loaded to failure to measure their fracture resistance. The data were analyzed using by two-way ANOVA and Tukey's HSD post-hoc test (α = 0.05). RESULTS: All specimens survived the aging protocols. The yttria content significantly affected the fracture resistance of the crowns (p < 0.0001). The mean fracture resistance, from highest to lowest: 3Y-PSZ, 4Y-PSZ, followed by the two multi-yttria-layered systems. The mean difference between the two multi-yttria-layered systems were not statistically significant (p = 0.98). The mechanical loading protocol did not affect the mean fracture resistance within each group (p = 0.18). CONCLUSIONS: Within each group, there was no difference in fracture resistance after thermocycling alone and thermo-mechanical loading. However, increasing the yttria concentration at the occlusal third of the crown decreased its fracture resistance. CLINICAL SIGNIFICANCE: The term "monolithic zirconia" alone without specifying the actual yttria content is misleading. This term represents different materials with different mechanical properties. The yttria content has an inverse relationship with the fracture resistance of zirconia crowns. The fracture resistance of multi-layer zirconia crowns is determined by the amount of the weaker zirconia phase at the occlusal part of the restoration rather than enforced by the stronger zirconia at the cervical part of the crown.

Composition, processing, and properties of biphasic zirconia bioceramics: relationship to competing strength and optical properties.

A study is made of relationships between composition, processing, structure and properties of biphasic zirconia bioceramics. The focus is on zirconia compositions with different yttria dopant contents used in modern dental restorations, namely 3 - 5 mol% yttria stabilized zirconia (3YSZ, 4YSZ, and 5YSZ). Crystallographies and densities are surveyed, sintering conditions examined, and microstructures characterized. Strength and optical tests are conducted on each YSZ, and dependencies on sintering temperature, cubic content and grain size analyzed. Strength correlates with the amount of tetragonal zirconia (t-ZrO2) crystals with large lattice distortions (tetragonality). YSZ translucency correlates with content of cubic zirconia (c-ZrO2) and t-ZrO2 with low levels of tetragonality. Consistent with literature reporting, the materials rank in decreasing order 3YSZ, 4YSZ to 5YSZ for strength but increasing order for translucency. However, for a given composition, the data suggest that the strengths of densely sintered 3YSZ and 4YSZ actually increase with translucency, although that of 5YSZ remains undiminished. These trends are in apparent contradiction to prevailing experience, and offer potential future processing routes to optimization of clinical materials.

Nanocrevasse-Rich Carbon Fibers for Stable Lithium and Sodium Metal Anodes.

Metallic lithium (Li) and sodium (Na) anodes have received great attention as ideal anodes to meet the needs for high energy density batteries due to their highest theoretical capacities. Although many approaches have successfully improved the performances of Li or Na metal anodes, many of these methods are difficult to scale up and thus cannot be applied in the production of batteries in practice. In this work, we introduce nanocrevasses in a carbon fiber scaffold which can facilitate the penetration of molten alkali metal into a carbon scaffold by enhancing its wettability for Li/Na metal. The resulting alkali metal/carbon composites exhibit stable long-term cycling over hundreds of cycles. The facile synthetic method is enabled for scalable production using recycled metal waste. Thus, the addition of nanocrevasses to carbon fiber as a scaffold for alkali metals can generate environmentally friendly and cost-effective composites for practical electrode applications.

An unexpected large capacity of ultrafine manganese oxide as a sodium-ion battery anode.

MnO2 is shown for the first time to be electrochemically active as a conversion anode for Na-ion batteries (NIBs). Space-confined ultrafine (UF)-MnO2, with an average crystal size of 4 nm, synthesized using a porous silicon dioxide templated hydrothermal process exhibits a high reversible sodiation capacity of 567 mA h g(-1), in contrast to the negligible activity shown by the aggregates of larger (14 nm) MnO2 nanocrystallites. The remarkably enhanced sodiation activity of the UF-MnO2 is attributable to its greatly reduced crystal size, which facilitates diffusion of Na ions, along with high surface energy arising from extensive heterogeneous interfacial bonding with the SiO2 surrounding. The UF-MnO2 anode exhibits an exceptional rate and cycle performance, exhibiting >70% capacity retention after 500 cycles. In operando synchrotron X-ray absorption near-edge structural analysis reveals combined charge-storage mechanisms involving conversion reaction between Mn(III) and Mn(II) oxides, Mn(III)-O1.5 + Na(+) + e(-)- ↔ 1/2Na2O + Mn(II)-O, and non-Mn-centered redox reactions. The finding suggests a new strategy for "activating" the potential electrochemical electrode materials that appear inactive in the bulk form.