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Zirconia restorations, which are fabricated by additive 3D gel deposition and do not require glazing like conventional restorations, were introduced as “self-glazed” zirconia restorations into dentistry. This in vitro investigation characterized the surface layer, microstructure and the fracture and aging behavior of “self-glazed” zirconia (Y-TZPSG) three-unit fixed dental prostheses (FDP) and compared them to conventionally CAD/CAM milled and glazed controls (Y-TZPC-FDPs). For this purpose, the FDPs were analyzed by (focused ion beam) scanning electron microscopy, laserscanning microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction and a dynamic and static loading test. For the latter, half of the samples of each material group (n = 16) was subjected to 5 million cycles of thermocyclic loading (98N) in an aqueous environment in a chewing simulator. Afterwards, all FDPs were loaded to fracture. Y-TZPSG-FDPs demonstrated a comparable elemental composition but higher surface microstructural homogeneity and fracture strength compared to Y-TZPC-FDPs. Microstructural flaws within the FDPs’ surfaces were identified as fracture origins. The high fracture strength of the Y-TZPSG-FDPs was attributed to a finer-grained microstructure with fewer surface flaws compared to the Y-TZPC-FDPs which showed numerous flaws in the glaze overlayer. A decrease in fracture strength after dynamic loading from 5165N to 4507N was observed for the Y-TZPSG-FDPs, however, fracture strength remained statistically significantly above the one measured for Y-TZPC-FDPs (before chewing simulation: 1923N; after: 2041N). Within the limits of this investigation, it can therefore be concluded that Y-TZPSG appears to be stable for clinical application suggesting further investigations to prove clinical applicability.

ZrO2-based ceramics are widely used in biomedical applications due to its color, biocompatibility, and excellent mechanical properties. However, low-temperature degradation (LTD) introduces a potential risk for long-term reliability of these materials. The development of innovative nondestructive techniques, which can explore LTD in zirconia-derived compounds, is strongly required. Yttria stabilized zirconia, 3Y-TZP, is one of the well-developed ZrO2-based ceramics with improved resistance to LTD for dental crown and implant applications. Here, 3Y-TZP ceramic powders were pressed and sintered to study the LTD phenomenon by phase transition behavior. The LTD-driven tetragonal-to-monoclinic phase transition was confirmed by XRD. XPS analysis demonstrated that induced LTD reduced the oxygen vacancies which supports these findings. It is proved that after the degradation, the 3Y-TZP ceramics show the decreased dielectric permittivity at terahertz frequencies due to the crystallographic phase transformation. Terahertz nondestructive probe is a promising method to investigate LTD in zirconia ceramics.

Biocompatibility of yttria (3 mol%) stabilized zirconia ceramics, 3Y-TZP, was affected to a large degree as a result of protein adsorption from human saliva that in turn depends on materials surface properties. Variable nano-roughness levels in 3Y-TZP discs were characterized and tested for specificity and selectivity with respect to size and uptake for human salivary protein.

The behaviors of grain growth dominate the formation of the microstructure inside polycrystalline materials and thus strongly influence their practical performances. However, grain growth behaviors still remain ambiguous and thus lack a mathematical formula to describe the general evolution despite decades of efforts. Here, we propose a new migration model of grain boundary (GB) and further derive a mathematical expression to depict the general evolution of grain growth in the cellular structures. The expression incorporates the variables influencing growth rate (e.g. GB features, grain size and local grain size distribution) and thus reveals how the normal, abnormal and stagnant behaviors of grain growth occur in polycrystalline systems. In addition, our model correlates quantitatively GB roughening transition with grain growth behavior. The general growth theory may provide new insights into the GB thermodynamics and kinetics during the cellular structure evolution.

Stereolithography has been proven as a feasible approach to make crack-free ceramic macrostructure with customized designs, but the microstructure, especially pore structure remains to be tailored more precisely for better performance, where the sintering protocol and related densification characteristics could play a vital role as the slurry preparation and debinding protocol do. Herein we report a phenomenon named “asynchronous densification”, that is, the surface region of zirconia ceramics formed by stereolithographic additive manufacturing would be densified prior to the bulk at 1200°C during the conventional pressureless sintering in air. The cause of this asynchronism is unclear but supposed to be correlated with low packing density, high sintering activity, poor thermal conduction of ceramics and impurities. Early densification of the surface may have negative effects towards ceramic components with more homogeneous microstructure, suppressed pore coalescence and limited grain growth, and therefore needs to be better controlled through optimization in sintering protocol.

Bone mineral consists of calcium hydroxy-carbonate apatite (HCA) that incorporates other minor cation substituents, primarily Na+ (0.5-0.8 wt %). We examine the carbonate species in various HCA specimens with variable CO32- contents (4-10 wt %), encompassing phases prepared by precipitation and a biomimetic specimen formed from a bioactive glass inside a simulated body fluid as well as bone tissue from beagle dog. Using magic-angle spinning (MAS) nuclear magnetic resonance (NMR) along with infrared spectroscopy experiments, we identified and quantified carbonate anions replacing either hydroxyl (A-type CO32-) or phosphate (B-type CO32-) anions in the HCA lattice, along with the carbonate species present in the amorphous surface layer present at all synthetic and biogenic nanocrystalline HCA particles. Advanced C-13-based NMR experimentation enabled the selective detection of the minor (CO32-)-C-13 population of intact bone monoliths, whose C-13 NMR signals are otherwise swamped by those from collagen, unless chemically invasive deproteination procedures are invoked. The CO32- species present in 4 week- and 8 month-old bone of the alveolar process from beagle dog revealed mainly B-type lattice sites and carbonates present in the amorphous surface layer. No tissue aging effects were observed in the local CO32- environments. Likewise, NMR revealed very similar Na-23(+) parameters in HCA, regardless of its synthetic or biogenic origin or degree of structural order. A combination of interatomic-distance-sensitive MAS NMR experiments allowed the identification of the local environments of the various carbonate, phosphate, hydroxyl, and water species present in both the interior and the surface layer of the synthetic HCA particles. We highlight the similarities/differences in the chemical speciation and the spatial distribution of CO32- anions present in carbonate-bearing amorphous calcium phosphate (ACP) relative to the ACP-like surface layer of HCA and discuss the C-13 N

Ferroelectric domain walls (DWs) are important nanoscale interfaces between two domains. It is widely accepted that ferroelectric domain walls work idly at terahertz (THz) frequencies, consequently discouraging efforts to engineer the domain walls to create new applications that utilize THz radiation. However, the present work clearly demonstrates the activity of domain walls at THz frequencies in a lead-free Aurivillius phase ferroelectric ceramic, Ca0.99Rb0.005Ce0.005Bi2Nb2O9, examined using THz-time-domain spectroscopy (THz-TDS). The dynamics of domain walls are different at kHz and THz frequencies. At low frequencies, domain walls work as a group to increase dielectric permittivity. At THz frequencies, the defective nature of domain walls serves to lower the overall dielectric permittivity. This is evidenced by higher dielectric permittivity in the THz band after poling, reflecting decreased domain wall density. An elastic vibrational model has also been used to verify that a single frustrated dipole in a domain wall represents a weaker contribution to the permittivity than its counterpart within a domain. The work represents a fundamental breakthrough in understanding the dielectric contributions of domain walls at THz frequencies. It also demonstrates that THz probing can be used to read domain wall dielectric switching.

Among homologous series of metal oxides, Andersson-Magneli phases TinO2n-1 (n=4-10) have attracted renewed scientific attention because of their behaviour in electrical conductivity and chemical/thermal stability. Various applications have also been reported for the phases with different values of n, or slightly reduced rutile (TiO2). The characteristic properties of these materials depend strongly on the compositional deviation from TiO2 and the way in which the structure accommodates the deviation. Thus, an urgent requirement is to overcome difficulties in characterizing such materials at atomic resolution. Here, we trace the discovery of the Andersson-Magneli phases, and report the application of recent developments in electron microscopy to reveal the relation, at the local level, between structural characteristics and electronic states, specifically for the materials TinO2n-1 with n=4-8. The electrical conductivity of Ti4O7 has been reported previously to show three clearly distinct states on decreasing temperature from 300 K. For this reason, we focus on Ti4O7 as a representative example of the TinO2n-1 phases and report structural characteristics at temperatures corresponding to each of the three different phases, focusing on the distribution of Ti3+ and Ti4+ cations from analysis of single-crystal XRD data. Electron diffraction experiments and electrical conductivity measurements are also reported.

Grain growth plays a crucial role in developing the microstructures of polycrystalline materials during heating treatment. In this work, SrTiO3 ceramics sintered at different heating rates (10 degrees C/min and 100 degrees C/min) display the distinctly different grain growth behaviors and microstructures between them. The onset temperature of rapid grain growth and mechanical-performance-related fracture mode are apparently different between these two sets of samples. Two grain growth mechanisms are demonstrated to dominate separately the sintering of SrTiO3 nanocrystals at different heating rates, i.e. conventional mechanism of atom-by-atom additions for grain growth at 10 degrees C/min and ordered coalescence of nanocrystals for grain growth at 100 degrees C/min. It is demonstrated that the switch of growth mechanisms is determined by the competition between the activation of grain motions and the formation of steady neck among grains.

A fused deposition modeling(FDM)system via screw extrusion suitable for feeding granular feedstocks with high solid loading was developed. Key parameters included aspect ratio of the screw, the compression ratio and pitch etc. In order to get constant extruded mass flow and wire diameter a processing window was determined by optimizing the barrel temperature, the nozzle diameter and the screwing speed. Microstructural characterization coupled with flexural strength measurement revealed that a higher printing temperature was beneficial to the inter layer bonding. The sintered zirconia ceramic samples with 99% of theoretical density of the 3 mol% yttria stabilized tetragonal zirconia polycrystal (3Y-TZP) and flexural strength of 890 +/- 60 MPa was obtained. A set of zirconia ceramic parts with complex geometries and controllable dimensional accuracy was also successfully prepared for demonstrating the potential of the technique.

Phosphates particularly zinc phosphates is a family of conventional dental cements that was developed a century ago and has been in use until today despite the fact that a number of new resin composite cements have been introduced in the market through the years. A close inspection of thein vivoaged samples provides insides to the margins and to the micro-leakage thus would sharpen the understanding and inspire the future development of the cements and cementation interfaces between the dental restorations and the natural tooth or implant abutment. This study highlights the cementation interface and its structural change duringin vivoaging. Besides the focused studies on phosphate cements, limited investigation has also been performed on resin composite cements as references.

The surface profile roughness (Ra), surface area roughness (Sa), and surface topography of newly developed as-prepared, ground, and polished self-glazed zirconia (SGZ) were evaluated using a profilometer, 3D optical surface profiler, and SEM, with conventional dry-milled zirconia (CZ) as a reference. A statistical analysis was conducted using repeated measures analysis of variance (ANOVA) and the Bonferroni test (alpha = .05). Results revealed that the material (p = .005), clinical adjustment procedure (p < .001), and interaction between factors (p < .001) had statistically significant effects on the Ra values. SGZ showed lower Sa values than CZ during the same period. Ten patient cases involving the restoration of the monolithic anatomic contour SGZ crowns were investigated. All crowns remained functional until the latest clinical follow-up and no further antagonist wear was observed. Thus, SGZ had relatively lower surface roughness, which was also more easily altered than that of CZ.

Purpose: The aim of this in vitro study was to evaluate the three-dimensional trueness and margin quality of monolithic zirconia restorations fabricated by additive 3D gel deposition, compared with those by subtractive milling. Methods: Ten single crowns and ten 4-unit FPDs of different occlusal geometries and margin thickness were fabricated by additive 3D gel deposition (additive group) and subtractive milling (subtractive group). An intraoral scanner was used to digitalize the restorations. 3D deviation analysis was applied and root mean square (RMS) was used to assess the trueness. Margin quality was characterized using optical stereomicroscopy and 3D laser scanning microscopy. Results: For single crowns with shallow fossae and grooves and normal margin, RMS value of additive group and subtractive group showed no significant difference in external surface, while additive group showed higher RMS value in intaglio surface. As for 4-unit FPDs with deep fossae and grooves and thin margin, RMS value of additive group in external surface was significantly lower than that of subtractive group and in intaglio surface there was no significant difference between two groups. With a 0.5 mm chamfer design, single crowns in additive group showed flawless margin with a smooth contour line, whereas minor flaws could be observed in 4-unit FPDs with thin margin. In subtractive group, restorations showed minor flaws or defects of various number and severity. Conclusions: Monolithic zirconia restorations fabricated by additive 3D gel deposition have comparable trueness and better margin quality than those fabricated by subtractive milling. Besides it is more capable of enabling complex geometry.

Dense oxide dispersion strengthened (ODS) 316 L steels with different amount of Y2O3 additions were successfully fabricated by selective laser melting (SLM) even though part of the added Y2O3 got lost during the process. The microstructure was characterized in details and the mechanical properties were tested at room temperature, 250 degrees C and 400 degrees C, respectively. The effect of the scanning speed on agglomeration of nanoparticles during SLM process was discussed. Superior properties, e.g., yield strength of 574 MPa and elongation of 91%, were achieved at room temperature in SLM ODS 316 L with additional 1% of Y2O3. At elevated temperatures, the strength kept high but the elongations dropped dramatically. It was observed that nano-voids nucleated throughout the whole gauge section at the sites where nanoinclusions located. The growth and coalescence of these voids were suppressed by the formation of an element segregation network before necking, which relieved local stress concentration and thus delayed necking. This unusual necking behavior was studied and compared to the previous theory. It appeared that the strong convection presented in the melt pool can evenly redistribute the short-time milled coarse Y2O3 precursor powder during SLM process. These findings can not only solve the problems encountered during the fabrication of ODS components but also replenish the strengthening mechanism of SLM 316 L thus pave a way for further improving of mechanical properties.

As a divertor plasma-facing material, W will experience high-flux plasma irradiation. In particular, severe surface morphology change like fuzz formation can be induced by He plasma irradiation. In this study, fuzz formation on additively manufactured W and W-Ta was investigated. Rolled W, laser-powder-bed-fused (LPBFed) W and W-Ta were exposed to high flux (similar to 10(23) m(-2) s(-1)) He plasma in the linear plasma generator Magnum-PSI with ion energy 12-13 eV at 1273 K. The mean thickness of the fuzz at grain interiors of rolled W, LPBFed W and W-Ta was measured as 0.37 mu m, 0.71 mu m and 0.23 mu m, respectively. The fuzz suppression in LPBFed W-Ta can be attributed to the synergetic effect of solid-solution, dislocation, and secondary-phase nanoparticles. Abnormally grown fuzz was observed near the pre-existing cracks of LPBFed W, while no such structure was found in LPBFed W-Ta. It is found that dislocations play a crucial role in inhibiting fuzz growth. This is confirmed by the difference in fuzz structure in rolled W and LPBFed W, where rolled W has a much greater dislocation density compared to LPBFed W. This work suggests that the fuzz growth kinetics may be tuned by tailoring the microstructures using the LPBF technique.