An electron microscopy study of sintering in three dental porcelains

In the manufacture of yttria partially stabilised zirconia dental prostheses, layers of porcelain veneer are sintered onto zirconia copings in order to reduce surface hardness and to produce an aesthetically pleasing finish. The stress of this interfacial bond and of the near-interface porcelain layers is crucial for reducing the likelihood of chipping during use. An improved understanding of the sintering behavior and the resulting microstructure is therefore required to ensure good prosthesis performance. In this study we use scanning electron microscopy in combination with energy dispersive spectroscopy mapping to examine the impact of vacuum sintering on the microstructure and elemental distribution of three types IPS e.max® Ceram dental porcelain (Incisal, BI shade and C4 shade) over 400 x 400 pm2 regions. It was found that the powder samples showed distinct differences in the average grain size (7 - 16 pm), maximum grain size (12 - 33 pm) and elemental composition prior to sintering. Following the application of the recommended sintering regimes, clear differences could be observed between the three samples. The Incisal porcelain demonstrated a uniform surface with limited numbers of grains and no evidence for porosity. In contrast, large numbers of sodium, aluminum and calcium rich grains were observed on the surface of the shaded porcelains, along with clear evidence of voiding.".</p

Residual strain mapping through pair distribution function analysis of the porcelain veneer within a yttria partially stabilised zirconia dental prosthesis

OBJECTIVE: Residually strained porcelain is influential in the early onset of failure in Yttria Partially Stabilised Zirconia (YPSZ) - porcelain dental prosthesis. In order to improve current understanding it is necessary to increase the spatial resolution of residual strain analysis in these veneers. METHODS: Few techniques exist which can resolve residual stress in amorphous materials at the microscale resolution required. For this reason, recent developments in Pair Distribution Function (PDF) analysis of X-ray diffraction data of dental porcelain have been exploited. This approach has facilitated high-resolution (70μm) quantification of residual strain in a YPSZ-porcelain dental prosthesis. In order to cross-validate this technique, the sequential ring-core focused ion beam and digital image correlation approach was implemented at a step size of 50μm. This semi-destructive technique exploits microscale strain relief to provide quantitative estimates of the near-surface residual strain. RESULTS: The two techniques were found to show highly comparable results. The residual strain within the veneer was found to be primarily tensile, with the highest magnitude stresses located at the YPSZ-porcelain interface where failure is known to originate. Oscillatory tensile and compressive stresses were also found in a direction parallel to the interface, likely to be induced by the multiple layering used during fabrication. SIGNIFICANCE: This study provides the insights required to improve prosthesis modelling, to develop new processing routes that minimise residual stress and ultimately to reduce prosthesis failure rates. The PDF approach also offers a powerful new technique for microscale strain quantification in amorphous materials.</p

Microscale resolution fracture toughness profiling at the zirconia-porcelain interface in dental prostheses

The high failure rate of the Yttria Partially Stabilized Zirconia (YPSZ)-porcelain interface in dental prostheses is influenced by the micro-scale mechanical property variation in this region. To improve the understanding of this behavior, micro-scale fracture toughness profiling by nanoindentation micropillar splitting is reported for the first time. Sixty 5 μm diameter micropillars were machined within the first 100 μm of the interface. Berkovich nanoindentation provided estimates of the bulk fracture toughness of YPSZ and porcelain that matched the literature values closely. However, the large included tip angle prevented precise alignment of indenter with the pillar center. Cube corner indentation was performed on the remainder of the pillars and calibration between nanoindentation using different tip shapes was used to determine the associated conversion factors. YPSZ micropillars failed by gradual crack propagation and bulk values persisted to within 15 μm from the interface, beyond which scatter increased and a 10% increase in fracture toughness was observed that may be associated with grain size variation at this location. Micropillars straddling the interface displayed preferential fracture within porcelain parallel to the interface at a location where nano-voiding has previously been observed and reported. Pure porcelain micropillars exhibited highly brittle failure and a large reduction of fracture toughness (by up to ∼90%) within the first 50 μm of the interface. These new insights constitute a major advance in understanding the structure-property relationship of this important bi-material interface at the micro-scale, and will improve micromechanical modelling needed to optimize current manufacturing routes and reduce failure.</p

Full in-plane strain tensor analysis using the microscale ring-core FIB milling and DIC approach

Microscale Full In-plane Strain Tensor (FIST) analysis is crucial for improving understanding of residual stress and mechanical failure in many applications. This study outlines the first Focused Ion Beam (FIB) milling and Digital Image Correlation (DIC) based technique capable of performing precise, reliable and rapid quantification of this behaviour. The nature of semi-destructive FIB milling overcomes the main limitations of X-Ray Diffraction (XRD) strain tensor quantification: unstrained lattice parameter estimates are not required, analysis is performed in within a precisely defined 3D microscale volume, both amorphous and crystalline materials can be studied and access to X-ray/neutron facilities is not required. The FIST FIB milling and DIC experimental technique is based on extending the ring-core milling geometry to quantify the strain variation with angle and therefore benefits from the excellent precision and simple analytical approach associated with this method. In this study in-plane strain analysis was performed on sample of commercial interest: a porcelain veneered Yttria Partially Stabilised Zirconia (YPSZ) dental prosthesis, and was compared with the results of XRD. The two methods sample different gauge volumes and mechanical states: approximately plane stress for ring-core milling, and a through-thickness average for XRD. We demonstrate using complex analysis methods and Finite Element (FE) modelling that valid comparisons can be drawn between these two stress states. Excellent agreement was obtained between principal stress orientation and magnitudes, leading to realistic residual stress estimates that agree well with the literature (. As a measure of validity of the matching approach we report the upper and lower bounds on the (101) interplanar spacing of YPSZ that are found to correspond to the range Å , closely matching published values

A comparative transmission electron microscopy, energy dispersive x-ray spectroscopy and spatially resolved micropillar compression study of the yttria partially stabilised zirconia - Porcelain interface in dental prosthesis

Recent studies into the origins of failure of yttria partially stabilised zirconia-porcelain veneered prosthesis have revealed the importance of micro-to-nano scale characterisation of this interface zone. Current understanding suggests that the heat treatment, residual stresses and varying microstructure at this location may contribute to near-interface porcelain chipping. In this study the chemical, microstructural and mechanical property variation across the interfacial zone has been characterised at two differing length scales and using three independent techniques; energy dispersive X-ray spectroscopy, transmission electron microscopy and micropillar compression. Energy dispersive X-ray spectroscopy mapping of the near-interface region revealed, for the first time, that the diffusional lengths of twelve principal elements are limited to within 2-6 μm of the interface. This study also revealed that 0.2-2 μm diameter zirconia grains had become detached from the bulk and were embedded in the near-interface porcelain. Transmission electron microscopy analysis demonstrated the presence of nanoscale spherical features, indicative of tensile creep induced voiding, within the first 0.4-1.5 μm from the interface. Within zirconia, variations in grain size and atomistic structure were also observed within the 3 μm closest to the interface. Micropillar compression was performed over a 100 μm range on either side of the interface at the spatial resolution of 5 μm. This revealed an increase in zirconia and porcelain loading modulus at close proximities (&lt; 5 μm) to the interface and a decrease in zirconia modulus at distances between 6 and 41 μm from this location. The combination of the three experimental techniques has revealed intricate details of the microstructural, chemical and consequently mechanical heterogeneities in the YPSZ-porcelain interface, and demonstrated that the length scales typically associated with this behaviour are approximately ± 5 μm.</p

‘High risk’ clinical and inflammatory clusters in COPD of Chinese descent

This is the author accepted manuscript. The final version is available from Elsevier via the DOI in this recordIntroduction COPD is a heterogeneous disease demonstrating inter-individual variation. A high COPD prevalence in Chinese populations is described but little is known about disease clusters and prognostic outcomes in the Chinese population across South-East Asia. We aim to determine if clusters of Chinese patients with COPD exist and their association with systemic inflammation and clinical outcomes. Methods Chinese patients with stable COPD were prospectively recruited into two cohorts (derivation and validation) from six hospitals across three South-East Asian countries (Singapore, Malaysia and Hong Kong; n=1,480). Each patient was followed over two-years. Clinical data (including co-morbidities) were employed in unsupervised hierarchical clustering (followed by validation) to determine the existence of patient clusters and their prognostic outcome. Accompanying systemic cytokine assessments were performed in a subset (n=336) of COPD patients to determine if inflammatory patterns and associated networks characterised the derived clusters. Results Five patient clusters were identified including (1) Ex-tuberculosis (2) Diabetic (3) Low co-morbidity: low-risk (4) Low co-morbidity: high-risk and (5) cardiovascular. The ‘cardiovascular’ and ‘ex-tuberculosis’ clusters demonstrate highest mortality (independent of GOLD assessment) and illustrate diverse cytokine patterns with complex inflammatory networks. Conclusions We describe novel ‘clusters’ of Chinese COPD patients, two of which represent ‘high-risk’ clusters. The ‘cardiovascular’ and ‘ex-tuberculosis’ patient clusters exhibit high mortality, significant inflammation and complex cytokine networks. Clinical and inflammatory risk stratification of Chinese patients with COPD should be considered for targeted intervention to improve disease outcomes.Singapore Ministry of Health - National Medical Research CouncilSingapore Ministry of EducationNanyang Technological University, SingaporeEngineering and Physical Sciences Research Council (EPSRC

Autophagy governs protumorigenic effects of mitotic slippage-induced senescence

The most commonly utilized class of chemotherapeutic agents administered as a first-line therapy are antimitotic drugs; however, their clinical success is often impeded by chemoresistance and disease relapse. Hence, a better understanding of the cellular pathways underlying escape from cell death is critical. Mitotic slippage describes the cellular process where cells exit antimitotic drug-enforced mitotic arrest and "slip" into interphase without proper chromosome segregation and cytokinesis. The current report explores the cell fate consequence following mitotic slippage and assesses a major outcome following treatment with many chemotherapies, therapy-induced senescence. It was found that cells postslippage entered senescence and could impart the senescence-associated secretory phenotype (SASP). SASP factor production elicited paracrine protumorigenic effects, such as migration, invasion, and vascularization. Both senescence and SASP factor development were found to be dependent on autophagy. Autophagy induction during mitotic slippage involved the autophagy activator AMPK and endoplasmic reticulum stress response protein PERK. Pharmacologic inhibition of autophagy or silencing of autophagy-related ATG5 led to a bypass of G1 arrest senescence, reduced SASP-associated paracrine tumorigenic effects, and increased DNA damage after S-phase entry with a concomitant increase in apoptosis. Consistent with this, the autophagy inhibitor chloroquine and microtubule-stabilizing drug paclitaxel synergistically inhibited tumor growth in mice. Sensitivity to this combinatorial treatment was dependent on p53 status, an important factor to consider before treatment.Implications: Clinical regimens targeting senescence and SASP could provide a potential effective combinatorial strategy with antimitotic drugs.NRF (Natl Research Foundation, S’pore)MOE (Min. of Education, S’pore)Accepted versio