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.

Electron probe microanalysis (EPMA) is based on the comparison of characteristic intensities induced by monoenergetic electrons. When the electron beam ionizes inner atomic shells and these ionizations cause the emission of characteristic X-rays, secondary fluorescence can occur, originating from ionizations induced by X-ray photons produced by the primary electron interactions. As detectors are unable to distinguish the origin of these characteristic X-rays, Monte Carlo simulation of radiation transport becomes a determinant tool in the study of this fluorescence enhancement. In this work, characteristic secondary fluorescence enhancement in EPMA has been studied by using the splitting routines offered by PENELOPE 2008 as a variance reduction alternative. This approach is controlled by a single parameter NSPLIT, which represents the desired number of X-ray photon replicas. The dependence of the uncertainties associated with secondary intensities on NSPLIT was studied as a function of the accelerating voltage and the sample composition in a simple binary alloy in which this effect becomes relevant. The achieved efficiencies for the simulated secondary intensities bear a remarkable improvement when increasing the NSPLIT parameter; although in most cases an NSPLIT value of 100 is sufficient, some less likely enhancements may require stronger splitting in order to increase the efficiency associated with the simulation of secondary intensities.

A simple model is proposed to account for the loss of collected X-ray signal by the shadowing of X-ray detectors in the scanning transmission electron microscope. The model is intended to aid the analysis of three-dimensional elemental data sets acquired using energy-dispersive X-ray tomography methods where shadow-free specimen holders are unsuitable or unavailable. The model also provides a useful measure of the detection system geometry.

Scanning electron microscopy (SEM) of nanoscale objects in dry and fully hydrated conditions at different temperatures is of critical importance in revealing details of their interactions with an ambient environment. Currently available WETSEM capsules are equipped with thin electron-transparent membranes and allow imaging of samples at atmospheric pressure, but do not provide temperature control over the sample. Here, we developed and tested a thermoelectric cooling/heating setup for WETSEM capsules to allow ambient pressure in situ SEM studies with a temperature range between −15 and 100°C in gaseous, liquid, and frozen conditions. The design of the setup also allows for correlation of the SEM with optical microscopy and spectroscopy. As a demonstration of the possibilities of the developed approach, we performed real-time in situ microscopy studies of water condensation on a surface of Morpho sulkowskyi butterfly wing scales. We observed that initial water nucleation takes place on top of the scale ridges. These results confirmed earlier discovery of a preexisting polarity gradient of the ridges of Morpho butterflies. Our developed thermoelectric cooling/heating setup for environmental capsules meets the diverse needs for in situ nanocharacterization in material science, catalysis, microelectronics, chemistry, and biology.

A resolution metric intended for resolution analysis of arbitrary spatially calibrated images is presented. By fitting a simple sigmoidal function to pixel intensities across slices of an image taken perpendicular to light–dark edges, the mean distance over which the light–dark transition occurs can be determined. A fixed multiple of this characteristic distance is then reported as the image resolution. The prefactor is determined by analysis of scanning transmission electron microscope high-angle annular dark field images of Si<110>. This metric has been applied to optical, scanning electron microscope, and helium ion microscope images. This method provides quantitative feedback about image resolution, independent of the tool on which the data were collected. In addition, our analysis provides a nonarbitrary and self-consistent framework that any end user can utilize to evaluate the resolution of multiple microscopes from any vendor using the same metric.

This study examines the use of reflectivity-height transformation in full-field angle-deviation microscopes (ADM). In such microscopes, two light intensity distribution images of a prism’s total internal reflection and critical angle are obtained separately with two charge-coupled devices (CCDs), and are converted into a reflectivity profile point-to-point and then into angle of deviation matrix after the beam is reflected by the test sample; finally, the surface height of the sample is found through the triangular geometrical relationship. This method obtains the image through the effective imaging area of CCD. Once the two-dimensional (2D) image is obtained, the third dimension, height, is added to create a full-field 3D surface profile. Its conversion process is nonlinear; therefore, compensation must be made to reduce measurement errors. The optical magnification of high vertical resolution full-field 3D reflection-type ADM could reach >250 times, thus providing submicron measurements with nanometer vertical resolution and allowing for the simultaneous measurement of 2D and 3D images. Small defects on both transparent and nontransparent surfaces can be rapidly detected.