Sodium-activated calcium bentonite is used as a binder in iron ore pellets and is known to increase strength of both wet and dry iron ore green pellets. In this article, the microstructure of bentonite in magnetite pellets is revealed for the first time using scanning electron microscopy. The microstructure of bentonite in wet and dry iron ore pellets, as well as in distilled water, was imaged by various imaging techniques (e.g., imaging at low voltage with monochromatic and decelerated beam or low loss backscattered electrons) and cryogenic methods (i.e., high pressure freezing and plunge freezing in liquid ethane). In wet iron ore green pellets, clay tactoids (stacks of parallel primary clay platelets) were very well dispersed and formed a voluminous network occupying the space available between mineral particles. When the pellet was dried, bentonite was drawn to the contact points between the particles and formed solid bridges, which impart strength to the solid compact.

The recently developed in-column monochromators make it possible to record energy-c spectra with resolutions better than 30 meV from nanometer-sized regions. It should therefore in principle be possible to detect localized vibrational excitations. The scattering geometry in the electron microscope means that bond stretching in the specimen plane or longitudinal optic phonons dominate the scattering. Most promising for initial studies are vibrations with energies between 300 and 400 meV from hydrogen bonded to other atoms. Estimates of the scattering cross-sections on the basis of a simple model show that they are about the same as inner shell scattering cross-sections. Cross-sections also increase with charge transfer between the atoms, and theory incorporating realistic charge distributions shows that signal/noise is the only limitation to high-resolution imaging. Given the magnitude of the scattering cross-sections, minimizing the tail of the zero-loss peak is just as important as achieving a small-width at half-maximum. Improvements in both resolution and controlling the zero-loss tail will be necessary before it is practical to detect optic phonons in solids between 40 and 60 meV.

This study evaluated the effect of fluoride solutions on surface roughness and morphology of composites in the short and long term. Specimens were randomly assigned to experimental groups (n=5) according to type of composite (nanofilled, microhybrid, microfilled) and immersion media (artificial saliva, 0.05% sodium fluoride solution, Fluordent Reach, Oral-B, and Fluorgard). Roughness was evaluated at time intervals: T0 after 24 h in artificial saliva (baseline); T60 after being in assigned immersion media for 1 min daily over 60 days; and Tfinal after artificial aging (20,000 thermal cycles, 1,200,000 mechanical loading cycles, and continuous immersion for 1,825 min). Surface morphology was qualitatively analyzed by scanning electron microscopy (SEM) at T60 and Tfinal. Roughness data were submitted to analysis of variance for mixed repeated measures, Sidak, and Tukey tests at α=0.05. Micro-filled resin showed the highest roughness values. Fluoride solutions had no influence on roughness. Higher roughness values were observed after artificial aging. In SEM observations after the artificial aging, the specimens showed surface degradation, irrespective of immersion medium or type of composite. Nano-filled resin showed higher loss of resin matrix and protrusion of filler particles. Roughness was not influenced by fluoride solutions; however, it is material dependent and increases over time.

The classical implementation for putting quantitative figures on maps to reveal elemental compositions in transmission electron microscopy is by analytical methods like X-ray and energy-loss spectroscopy. Typically, the technique in use often depends on whether lighter or heavier elements are present and—more practically—which calibrations are available or sample-related properties are known. A framework linking electron energy-loss spectroscopy (EELS) and energy-dispersive X-ray (EDX) signals such that absolute volumetric concentrations can be derived without assumptions made a priori about the unknown sample, is largely missing. In order to combine both techniques and harness their respective potentials for a light and heavy element analysis, we have set up a powerful hardware configuration and implemented an experimental approach, which reduces the need for estimates on many parameters needed for quantitative work such as densities, absolute thicknesses, theoretical ionization cross-sections, etc. Calibrations on specimens with known geometry allow the measurement of inelastic mean free paths. As a consequence, mass-thicknesses obtained from the EDX ζ-factor approach can be broken up and quantities like concentrations and partial energy-differential ionization cross-sections become accessible. ζ-factors can then be used for conversion into EELS cross-sections that are hard to determine otherwise, or conversely, connecting EDXS and EELS in a quantitative manner quite effectively.

The resonant frequency and sensitivity of an atomic force microscope (AFM) with an assembled cantilever probe (ACP) is analyzed utilizing strain gradient theory, and then the governing equation and boundary conditions are derived by a combination of the basic equations of strain gradient theory and Hamilton’s principle. The resonant frequency and sensitivity of the proposed AFM microcantilever are then obtained numerically. The proposed ACP includes a horizontal cantilever, two vertical extensions, and two tips located at the free ends of the extensions that form a caliper. As one of the extensions is located between the clamped and free ends of the AFM microcantilever, the cantilever is modeled as two beams. The results of the current model are compared with those evaluated by both modified couple stress and classical beam theories. The difference in results evaluated by the strain gradient theory and those predicted by the couple stress and classical beam theories is significant, especially when the microcantilever thickness is approximately the same as the material length-scale parameters. The results also indicate that at the low values of contact stiffness, scanning in the higher cantilever modes decrease the accuracy of the proposed AFM ACP.

Scanning electron microscopy, focused ion beam (FIB), and transmission electron microscopy are combined to study the intergrowth of 90° rotational components and of ramps in coffin-shaped ZSM-5 crystals. The 90° rotational boundaries with local zig-zag features between different intergrowth components are observed in the main part of crystal. Also a new kind of displacement boundary is described. At the displacement boundary there is a shift of the unit cells along the boundary without a change in orientation. Based on lamellae prepared with FIB from different positions of the ramps and crystal, the orientation relationships between ramps and the main part of the crystal are studied and the three-dimensional morphology and growth mechanism of the ramp are illustrated.

Cold atom electron and ion sources produce electron bunches and ion beams by photoionization of laser-cooled atoms. They offer high coherence and the potential for high brightness, with applications including ultra-fast electron-diffractive imaging of dynamic processes at the nanoscale. The effective brightness of electron sources has been limited by nonlinear divergence caused by repulsive interactions between the electrons, known as the Coulomb explosion. It has been shown that electron bunches with ellipsoidal shape and uniform density distribution have linear internal Coulomb fields, such that the Coulomb explosion can be reversed using conventional optics. Our source can create bunches shaped in three dimensions and hence in principle achieve the transverse spatial coherence and brightness needed for picosecond-diffractive imaging with nanometer resolution. Here we present results showing how the shaping capability can be used to measure the spatial coherence properties of the cold electron source. We also investigate space-charge effects with ions and generate electron bunches with durations of a few hundred picoseconds. Future development of the cold atom electron and ion source will increase the bunch charge and charge density, demonstrate reversal of Coulomb explosion, and ultimately, ultra-fast coherent electron-diffractive imaging.

Scanning transmission electron microscopy (STEM) of specimens in liquid, so-called Liquid STEM, is capable of imaging the individual subunits of macromolecular complexes in whole eukaryotic cells in liquid. This paper discusses this new microscopy modality within the context of state-of-the-art microscopy of cells. The principle of operation and equations for the resolution are described. The obtained images are different from those acquired with standard transmission electron microscopy showing the cellular ultrastructure. Instead, contrast is obtained on specific labels. Images can be recorded in two ways, either via STEM at 200 keV electron beam energy using a microfluidic chamber enclosing the cells, or via environmental scanning electron microscopy at 30 keV of cells in a wet environment. The first series of experiments involved the epidermal growth factor receptor labeled with gold nanoparticles. The labels were imaged in whole fixed cells with nanometer resolution. Since the cells can be kept alive in the microfluidic chamber, it is also feasible to detect the labels in unfixed, live cells. The rapid sample preparation and imaging allows studies of multiple whole cells.

This aim of this study was to assess the discriminatory value of fractal and grey level co-occurrence matrix (GLCM) analysis methods in standard microscopy analysis of two histologically similar brain white mass regions that have different nerve fiber orientation. A total of 160 digital micrographs of thionine-stained rat brain white mass were acquired using a Pro-MicroScan DEM-200 instrument. Eighty micrographs from the anterior corpus callosum and eighty from the anterior cingulum areas of the brain were analyzed. The micrographs were evaluated using the National Institutes of Health ImageJ software and its plugins. For each micrograph, seven parameters were calculated: angular second moment, inverse difference moment, GLCM contrast, GLCM correlation, GLCM variance, fractal dimension, and lacunarity. Using the Receiver operating characteristic analysis, the highest discriminatory value was determined for inverse difference moment (IDM) (area under the receiver operating characteristic (ROC) curve equaled 0.925, and for the criterion IDM≤0.610 the sensitivity and specificity were 82.5 and 87.5%, respectively). Most of the other parameters also showed good sensitivity and specificity. The results indicate that GLCM and fractal analysis methods, when applied together in brain histology analysis, are highly capable of discriminating white mass structures that have different axonal orientation.

High-resolution radial distribution functions of as-implanted and thermally relaxed amorphous silicon created by ion implantation were measured using tilted-illumination selected area electron diffraction at room temperature. The diffracted intensities were measured out to a maximum scattering vector 2 sin(θ)/λ of 3.3–3.7 Å−1. The volume-averaged pair-correlation statistics of as-implanted and relaxed ion-implanted amorphous silicon are virtually indistinguishable with coordination numbers of 3.7 ± 0.3 and 3.9 ± 0.3 (for neighbors closer than 3 Å) and average bond angles of 109 ± 0.5° and 110 ± 0.6°, respectively. The atomic rearrangements in ion-implanted amorphous silicon due to a low temperature anneal are subtle.

Atomic force microscopy (AFM) and laser scanning microscopy (LSM) measurements on a series of specially designed roughness artifacts were performed and the results characterized by spectral analysis. As demonstrated by comparisons, both AFM and LSM can image the complex structures with high resolution and fidelity. When the surface autocorrelation length increases from 200 to 500 nm, the cumulative power spectral density spectra of the design, AFM and LSM data reach a better agreement with each other. The critical wavelength of AFM characterization is smaller than that of LSM, and the gap between the measured and designed critical wavelengths is reduced with an increase in the surface autocorrelation length. Topography measurements of surfaces with a near zero or negatively skewed height distribution were determined to be accurate. However, obvious discrepancies were found for surfaces with a positive skewness owing to more severe dilations of either the solid tip of the AFM or the laser tip of the LSM. Further surface parameter evaluation and template matching analysis verified that the main distortions in AFM measurements are tip dilations while those in LSM are generally larger and more complex.

This study demonstrates the accumulation of electron-induced secondary electrons by utilizing a simple geometrical configuration of two branches of a charged insulating biomaterial. The collective motion of these secondary electrons between the branches has been visualized by analyzing the reconstructed amplitude images obtained using in situ electron holography. In order to understand the collective motion of secondary electrons, the trajectories of these electrons around the branches have also been simulated by taking into account the electric field around the charged branches on the basis of Maxwell’s equations.

The characterization of biological and inorganic materials by determining their three-dimensional structure in conditions closer to their native state is a major challenge of technological research. Environmental scanning electron microscopy (ESEM) provides access to the observation of hydrated samples in water environments. Here, we present a specific device for ESEM in the scanning transmission electron microscopy mode, allowing the acquisition of tilt-series suitable for tomographic reconstructions. The resolution which can be obtained with this device is first determined. Then, we demonstrate the feasibility of tomography on wet materials. The example studied here is hydrophilic mesoporous silica (MCM-41). Finally, the minimum thickness of water which can be detected is calculated from Monte Carlo simulations and compared with the resolution expected in the tomograms.