Direct three-dimensional observation of the microstructure and chemistry of C3S hydration.

Disagreements about the mechanisms of cement hydration remain despite the fact that portland cement has been studied extensively for over 100 years. One reason for this is that direct observation of the change in microstructure and chemistry are challenging for many experimental techniques. This paper presents results from synchrotron nano X-ray tomography and fluorescence imaging. The data show unprecedented direct observations of small collections of C3S particles before and after different periods of hydration in 15 mmol/L lime solution. X-ray absorption contrast is used to make three dimensional maps of the changes of these materials with time. The chemical compositions of hydration products are then identified with X-ray fluorescence mapping and scanning electron microscopy. These experiments are used to provide insight into the rate and morphology of the microstructure formation.

Direct Measurements of 3D Structure, Chemistry and Mass Density During the Induction Period of C3S Hydration.

The reasons for the start and end of the induction period of cement hydration remain topic of controversy. One long-standing hypothesis is that a thin metastable hydrate forming on the surface of cement grains significantly reduces the particle dissolution rate; the eventual disappearance of this layer re-establishes higher dissolution rates at the beginning of the acceleration period. However, the importance, or even the existence, of this metastable layer has been questioned because it cannot be directly detected in most experiments. In this work, a combined analysis using nano-tomography and nano-X-ray fluorescence makes the direct imaging of early hydration products possible. These novel X-ray imaging techniques provide quantitative measurements of 3D structure, chemical composition, and mass density of the hydration products during the induction period. This work does not observe a low density product on the surface of the particle, but does provide insights into the formation of etch pits and the subsequent hydration products that fill them.

Residual thermal stress simulation in three-dimensional molar crown systems: a finite element analysis.

PURPOSE: To simulate coefficient of thermal expansion (CTE)-generated stress fields in monolithic metal and ceramic crowns, and CTE mismatch stresses between metal, alumina, or zirconia cores and veneer layered crowns when cooled from high temperature processing. MATERIALS AND METHODS: A 3D computer-aided design model of a mandibular first molar crown was generated. Tooth preparation comprised reduction of proximal walls by 1.5 mm and of occlusal surfaces by 2.0 mm. Crown systems were monolithic (all-porcelain, alumina, metal, or zirconia) or subdivided into a core (metallic, zirconia, or alumina) and a porcelain veneer layer. The model was thermally loaded from 900°C to 25°C. A finite element mesh of three nodes per edge and a first/last node interval ratio of 1 was used, resulting in approximately 60,000 elements for both solids. Regions and values of maximum principal stress at the core and veneer layers were determined through 3D graphs and software output. RESULTS: The metal-porcelain and zirconia-porcelain systems showed compressive fields within the veneer cusp bulk, whereas alumina-porcelain presented tensile fields. At the core/veneer interface, compressive fields were observed for the metal-porcelain system, slightly tensile for the zirconia-porcelain, and higher tensile stress magnitudes for the alumina-porcelain. Increasingly compressive stresses were observed for the metal, alumina, zirconia, and all-porcelain monolithic systems. CONCLUSIONS: Variations in residual thermal stress levels were observed between bilayered and single-material systems due to the interaction between crown configuration and material properties.

Mapping the tetragonal to monoclinic phase transformation in zirconia core dental crowns.

OBJECTIVE: Chipping failures observed clinically in bilayer systems of porcelain and zirconia restorations should be coupled with a monoclinic to tetragonal phase transformation in the zirconia layer due to the high compressive stress. METHODS: Phase transformations were mapped using 2D micro X-ray diffraction of 1083 frames at 100µm×100µm spacing automatically positioned along the core layer of a sectioned fractured crown. RESULTS: Yttria-zirconia tetragonal phase transformations to monoclinic zirconia and monoclinic yttria were observed, mostly at the impacted area. A simple map of (101) tetragonal d-spacing strain reveals stress relaxation during phase transformation was detected at inner section of lingual side, because the initial state of compressive residual stress assists this phase transformation at the inter section of lingual side of the core while initial tensile stress at the outer sides under the veneer relaxes under compression and initially prevents phase transformation. SIGNIFICANCE: This study implements an experimental method to map the phase transformation, after applying local compressive load until fracture. Such fractures resemble clinically observed chipping failure.