This paper shows that pair-distribution function (PDF) analyses can be carried out on organic and organometallic compounds from powder electron diffraction data. Different experimental setups are demonstrated, including selected area electron diffraction and nanodiffraction in transmission electron microscopy or nanodiffraction in scanning transmission electron microscopy modes. The methods were demonstrated on organometallic complexes (chlorinated and unchlorinated copper phthalocyanine) and on purely organic compounds (quinacridone). The PDF curves from powder electron diffraction data, called ePDF, are in good agreement with PDF curves determined from X-ray powder data demonstrating that the problems of obtaining kinematical scattering data and avoiding beam damage of the sample are possible to resolve.

Leaves of Anacardium humile are used in Brazilian traditional medicine for the treatment of intestinal disturbances and skin lesions. This study aimed to define leaf diagnostic structural characters, to propose a new method of phytochemical analysis of secretions, prospect flavonoids and alkaloids, and to evaluate their inhibitory activity on Candida albicans. Common anatomical, phytochemical, and microbiological methods were used. Leaves of Anacardium occidentale were used as a reference for the structural analyses. The main structural characters were closed vascular system, absence of ducts at the medulla, bilateral mesophyll, absence of bundle sheath extension, and secretory idioblasts at the xylem. The ducts present schizogenous origin, and secreting activity is restricted to the initial phases of leaf blade expansion. The proposed new phytochemical method is practical and inexpensive and has potential for wide application. The abundance of tannins and flavonoids is related to medicinal use. A single peak in high-performance liquid chromatography indicated the presence of a pure substance not previously reported. The extract had a strong inhibitory effect on C. albicans. The obtained results confirm the potential of A. humile for the prospection of new bioactive compounds.

Using an in situ load frame within a scanning electron microscope, a microstructural section on the surface of an annealed tantalum (Ta) polycrystalline specimen was mapped at successive tensile strain intervals, up to ~20% strain, using electron backscatter diffraction. A grain identification and correlation technique was developed for characterizing the evolving microstructure during loading. Presenting the correlated results builds on the reference orientation deviation (ROD) map concept where individual orientation measurements within a grain are compared with a reference orientation associated with that grain. In this case, individual orientation measurements in a deformed grain are measured relative to a reference orientation derived from the undeformed (initial) configuration rather than the current deformed configuration as has been done for previous ROD schemes. Using this technique helps reveal the evolution of crystallographic orientation gradients and development of deformation-induced substructure within grains. Although overall crystallographic texture evolved slowly during deformation, orientation spread within grains developed quickly. In some locations, misorientation relative to the original orientation of a grain exceeded 20° by 15% strain. The largest orientation changes often appeared near grain boundaries suggesting that these regions were preferred locations for the initial development of subgrains.

Changes in the ultrastructure and chemical components, and their distribution in Japanese beech (Fagus crenata), during the ionic liquid 1-ethylpyridinium bromide ([EtPy][Br]) treatment were examined at the cellular level by light microscopy, scanning electron microscopy, and confocal Raman microscopy. Each of the tissues, including wood fibers, vessels and parenchyma cells treated with [EtPy][Br] showed specific morphological characteristics. Furthermore, lignin can be preferentially liquefied and eluted in [EtPy][Br] from the cell walls when compared to polysaccharides. However, the delignification was heterogeneous on the cell walls as lignin maintained a relatively high-concentration at the compound middle lamella, cell corners, inner surface of the secondary wall, and pits after [EtPy][Br] treatment.

Micro energy-dispersive X-ray fluorescence spectrometry (µ-EDXRF) and scanning electron microscopy (SEM) were used to evaluate dentin treated with an etch and rinse adhesive (ER) and a self-etch adhesive (SE). Ten human molars (H) and ten bovine anterior teeth (B) were prepared (exposure of dentin and divided in the middle) and allocated into two different adhesion strategy groups per substrate (n=40). µ-EDXRF data and SEM images were obtained before and after treatment. Untreated dentin of both substrates did not differ in terms of Ca (p<0.1503), P (p<0.2986) or Ca/P ratio (p<0.1400). H-SE and B-SE specimens showed reduced P content (p<0.0001; p<0.0002), while H-ER and B-ER specimens showed reduced Ca and P content (p<0.0001; p<0.0001) when compared with untreated specimens. The Ca/P ratio was significantly higher in H-ER and B-ER specimens than in H-SE and B-SE specimens (p<0.0001; p<0.0080). Untreated dentin showed a homogeneous elemental distribution. However, after adhesive treatments, the surface of the dentin showed an irregular demineralization pattern. The resin tags and adhesive layer were shorter in bovine specimens than in human specimens due to morphological differences.

Combined tilt- and focal series scanning transmission electron microscopy is a recently developed method to obtain nanoscale three-dimensional (3D) information of thin specimens. In this study, we formulate the forward projection in this acquisition scheme as a linear operator and prove that it is a generalization of the Ray transform for parallel illumination. We analytically derive the corresponding backprojection operator as the adjoint of the forward projection. We further demonstrate that the matched backprojection operator drastically improves the convergence rate of iterative 3D reconstruction compared to the case where a backprojection based on heuristic weighting is used. In addition, we show that the 3D reconstruction is of better quality.

The inflammatory resorption of dental root apex (i.e., the process of removal of cementum and/or dentine through the activity of resorbing cells) may show different configurations and damage the apical root structure. As knowing the morphology of resorption areas of human teeth is essential for the success of endodontic treatments, we investigated the apical resorption by scanning electron microscopy, focusing on roots with granulomas. A total of 30 teeth (with penetrating carious lesions and chronic periapical lesions) were examined, the apical third of the roots were removed and analyzed to estimate periforaminal and foraminal resorption, shape and morphology of foramen resorption, centering of the periforaminal resorption area, and diameters of each apical foramen. Periforaminal resorption was present in all samples, whereas foraminal resorption was present in 92% of cases (mainly funnel shaped). Lacunae were observed in the foraminal resorption area with an average diameter of 35±14 μm. The major and minor diameters of the foramina in teeth with resorption were 443 and 313 μm, respectively (higher than in healthy teeth). This result indicates an expansion of the apical diameters caused by the pathology, which could encourage a different clinical instrumentation for these teeth.

Polyvinylidene chloride (PVDC) co-polymer resins are commonly formulated with a variety of solid additives for the purpose of processing or stabilization. A homogeneous distribution of these additives during handling and processing is important. The Dow Chemical Company developed a process to incorporate solid materials in latex form onto PVDC resin bead surfaces using a coagulation process. In this context, we present a method to characterize the distribution and thickness of these latex coatings. The difference in backscattered electron signal from the higher mean atomic number PVDC core and lower atomic number latex coating in conjunction with scanning electron microscopy (SEM) imaging using a range of accelerating voltages was used to characterize latex thickness and distribution across large numbers of beads quickly and easily. Monte Carlo simulations were used to quantitatively estimate latex thickness as a function of brightness in backscatter electron images. This thickness calibration was validated by cross-sectioning using a focused ion-beam SEM. Thicknesses from 100 nm up to about 1.3 µm can be determined using this method.

EBSDinterp is a graphic user interface (GUI)-based MATLAB® program to perform microstructurally constrained interpolation of nonindexed electron backscatter diffraction data points. The area available for interpolation is restricted using variations in pattern quality or band contrast (BC). Areas of low BC are not available for interpolation, and therefore cannot be erroneously filled by adjacent grains “growing” into them. Points with the most indexed neighbors are interpolated first and the required number of neighbors is reduced with each successive round until a minimum number of neighbors is reached. Further iterations allow more data points to be filled by reducing the BC threshold. This method ensures that the best quality points (those with high BC and most neighbors) are interpolated first, and that the interpolation is restricted to grain interiors before adjacent grains are grown together to produce a complete microstructure. The algorithm is implemented through a GUI, taking advantage of MATLAB®’s parallel processing toolbox to perform the interpolations rapidly so that a variety of parameters can be tested to ensure that the final microstructures are robust and artifact-free. The software is freely available through the CSIRO Data Access Portal (doi:10.4225/08/5510090C6E620) as both a compiled Windows executable and as source code.

We propose a framework for indexing of grain and subgrain structures in electron backscatter diffraction patterns of polycrystalline materials. We discretize the domain of a dynamical forward model onto a dense grid of orientations, producing a dictionary of patterns. For each measured pattern, we identify the most similar patterns in the dictionary, and identify boundaries, detect anomalies, and index crystal orientations. The statistical distribution of these closest matches is used in an unsupervised binary decision tree (DT) classifier to identify grain boundaries and anomalous regions. The DT classifies a pattern as an anomaly if it has an abnormally low similarity to any pattern in the dictionary. It classifies a pixel as being near a grain boundary if the highly ranked patterns in the dictionary differ significantly over the pixel’s neighborhood. Indexing is accomplished by computing the mean orientation of the closest matches to each pattern. The mean orientation is estimated using a maximum likelihood approach that models the orientation distribution as a mixture of Von Mises–Fisher distributions over the quaternionic three sphere. The proposed dictionary matching approach permits segmentation, anomaly detection, and indexing to be performed in a unified manner with the additional benefit of uncertainty quantification.

The purpose of this study was to evaluate if mechanical loading influences bioactivity and bond strength at the resin–dentin interface after bonding with Zn-doped etch-and-rinse adhesives. Dentin surfaces were subjected to demineralization by 37% phosphoric acid (PA) or 0.5 M ethylenediaminetetraacetic acid (EDTA). Single bond (SB) adhesive—3M ESPE—SB+ZnO particles 20 wt% and SB+ZnCl2 2 wt% were applied on treated dentin to create the groups PA+SB, SB+ZnO, SB+ZnCl2, EDTA+SB, EDTA+ZnO, and EDTA+ZnCl2. Bonded interfaces were stored in simulated body fluid for 24 h and tested or submitted to mechanical loading. Microtensile bond strength (MTBS) was assessed. Debonded dentin surfaces were studied by high-resolution scanning electron microscopy. Remineralization of the bonded interfaces was assessed by atomic force microscope imaging/nanoindentation, Raman spectroscopy/cluster analysis, and Masson’s trichrome staining. Load cycling (LC) produced reduction in MTBS in all PA+SB, and no change was encountered in EDTA+SB specimens, regardless of zinc doping. LC increased the mineralization and crystallographic maturity at the interface; a higher effect was noticed when using ZnO. Trichrome staining reflected a narrow demineralized dentin matrix after loading of dentin surfaces that were treated with SB-doped adhesives. This correlates with an increase in mineral platforms or plate-like multilayered crystals in PA or EDTA-treated dentin surfaces, respectively.