RESUMO
The Dual Imaging and Diffraction (DIAD) beamline at Diamond Light Source (Didcot, U.K.) implements a correlative approach to the dynamic study of materials based on concurrent analysis of identical sample locations using complementary X-ray modalities to reveal structural detail at various length scales. Namely, the underlying beamline principle and its practical implementation allow the collocation of chosen regions within the sample and their interrogation using real-space imaging (radiography and tomography) and reciprocal space scattering (diffraction). The switching between the two principal modes is made smooth and rapid by design, so that the data collected is interlaced to obtain near-simultaneous multimodal characterization. Different specific photon energies are used for each mode, and the interlacing of acquisition steps allows conducting static and dynamic experiments. Building on the demonstrated realization of this state-of-the-art approach requires further refining of the experimental practice, namely, the methods for gauge volume collocation under different modes of beam-sample interaction. To address this challenge, experiments were conducted at DIAD devoted to the study of human dental enamel, a hierarchical structure composed of hydroxyapatite mineral nanocrystals, as a static sample previously affected by dental caries (tooth decay) as well as under dynamic conditions simulating the process of acid demineralization. Collocation and correlation were achieved between WAXS (wide-angle X-ray scattering), 2D (radiographic), and 3D (tomographic) imaging. While X-ray imaging in 2D or 3D modes reveals real-space details of the sample microstructure, X-ray scattering data for each gauge volume provided statistical nanoscale and ultrastructural polycrystal reciprocal-space information such as phase and preferred orientation (texture). Careful registration of the gauge volume positions recorded during the scans allowed direct covisualization of the data from two modalities. Diffraction gauge volumes were identified and visualized within the tomographic data sets, revealing the underlying local information to support the interpretation of the diffraction patterns. The present implementation of the 4D microscopy paradigm allowed following the progression of demineralization and its correlation with time-dependent WAXS pattern evolution in an approach that is transferable to other material systems.
RESUMO
Human enamel is a hierarchical mineralized tissue with a two-level composite structure. Few studies have focused on the structure-mechanical property relationship and its link to the multi-scale architecture of human enamel, whereby the response to mechanical loading is affected not only by the rod distribution at micro-scale, but also strongly influenced by the mineral crystallite shape, and spatial arrangement and orientation. In this study, two complementary synchrotron X-ray diffraction techniques, wide and small angle X-ray scattering (WAXS/SAXS) were used to obtain multi-scale quantitative information about the structure and deformation response of human enamel to in situ uniaxial compressive loading. The apparent modulus was determined linking the external load and the internal strain in hydroxyapatite (HAp) crystallites. An improved multi-scale Eshelby model is proposed taking into account the two-level hierarchical structure of enamel. This framework has been used to analyse the experimental data for the elastic lattice strain evolution within the HAp crystals. The achieved agreement between the model prediction and experiment along the loading direction validates the model and suggests that the new multi-scale approach reasonably captures the structure-property relationship for the human enamel. The ability of the model to predict multi-directional strain components is also evaluated by comparison with the measurements. The results are useful for understanding the intricate relationship between the hierarchical structure and the mechanical properties of enamel, and for making predictions of the effect of structural alterations that may occur due to the disease or treatment on the performance of dental tissues and their artificial replacements.