We investigated an eclogitic gneiss from the Western Gneiss Region in Norway, which underwent subduction as part of Baltica lithosphere beneath Laurentia during the Scandian orogeny. Petrologic data indicate that the eclogite was deformed plastically at about 4 GPa and 800°C producing a strong macroscopic foliation and lineation. Whereas garnet remained largely stable during the retrograde uplift, omphacite was transformed statically into a symplectite consisting of lamellar diopside and plagioclase with more equant grains of hornblende and orthopyroxene. Measurements of the crystallographic preferred orientation with electron backscatter diffraction show that diopside and hornblende, as well as orthopyroxene, have a systematic orientation relationship with the macroscopic fabric, as well as the (presumed) orientation of the host omphacite. The orientation relationship between the chain silicates is very sharp with the crystallographic forms {100}, {010}, and ⟨001⟩ being parallel. Their bulk texture shows a maximum of ⟨001⟩ parallel to the lineation and girdles of {010} and {110} perpendicular to the lineation with maxima subparallel to the foliation corresponding to an L-type texture of the original omphacite and indicating constrictional strain with an additional component of pure shear/simple shear component.

Pole figures are often used to present crystal orientation data. The huge number of single orientation measurements acquired by electron backscatter diffraction (EBSD) poses a challenge for pole figure representation due to the large number of calculations required. This significantly reduces the speed at which the data may be rotated and affects the ability to switch between different projection types. In the present work, it will be shown that satisfactory representation of orientation data in different projection types can generally be achieved by an imaging of a spherical projection. With this approach, explicit calculation of the projections is no longer required, allowing for both real-time dataset rotation and real-time switching between all projection types relevant to materials science. The technique can be applied to any other directional property distribution, for example, not only for EBSD orientation presentation.

Uni- and biaxial tension deformation tests, with different degrees of deformation, have been done on AISI 430 (EN 1.4016) ferritic stainless steel samples, which had both different chemical compositions and had undergone different annealing treatments. The initial and deformed materials were characterized by using electron backscatter diffraction and backscatter electron imaging in a scanning electron microscope together with electron probe microanalysis. The correlation observed among the chemical compositions, annealing treatment, and strain level obtained after deformation is discussed.

The microstructural evolution of a cold drawn copper wire (reduction area of 38%) during primary recrystallization and grain growth was observed in situ by electron backscatter diffraction. Two thermal treatments were performed, and successive scans were acquired on samples undergoing heating from ambient temperature to a steady state of 200°C or 215°C. During a third in situ annealing, the temperature was continuously increased up to 600°C. Nuclei were observed to grow at the expense of the deformed microstructure. This growth was enhanced by the high stored energy difference between the nuclei and their neighbors (driving energy in recrystallization) and by the presence of high-angle grain boundaries of high mobility. In the early stages of growth, the nuclei twin and the newly created orientations continue to grow to the detriment of the strained copper. At high temperatures, the disappearance of some twins was evidenced by the migration of the incoherent twin boundaries. Thermal grooving of grain boundaries is observed at these high temperatures and affects the high mobile boundaries but tends to preserve the twin boundaries of lower energy. Thus, grooving may contribute to the twin vanishing.

The role of grain orientation and grain boundary misorientation on the formation of subcritical grain boundary cracks in creep of a conventionally cast nickel-based superalloy has been studied. The crystallographic orientations of the grains adjacent to grain boundaries normal to the tensile axis were measured using electron backscattered diffraction. The difference in the Schmid factor for the {111} ⟨112⟩ slip system between the grains was compared to the occurrence of grain boundary cracking. In addition, the difference in the amount of potential primary creep was calculated. The cracked grain boundaries were found to have a larger difference in Schmid factor, as well as a larger difference in potential primary creep, compared with uncracked grain boundaries.

Duplex stainless steels (DSS) may be defined as a category of steels with a two-phase ferritic–austenitic microstructure, which combines good mechanical and corrosion properties. However, these steels can undergo significant microstructural modification as a consequence of either thermo-mechanical treatments (ferrite decomposition, which causes σ- and χ-phase formation and nitride precipitation) or plastic deformation at room temperature [austenite transformation into strain-induced martensite (SIM)]. These secondary phases noticeably affect the properties of DSS, and therefore are of huge industrial interest. In the present work, SIM formation was investigated in a 2101 lean DSS. The material was subjected to cold rolling at various degrees of deformation (from 10 to 80% thickness reduction) and the microstructure developed after plastic deformation was investigated by electron backscattered diffraction, X-ray diffraction measurements, and hardness and magnetic tests. It was observed that SIM formed as a consequence of deformations higher than ~20% and residual austenite was still observed at 80% of thickness reduction. Furthermore, a direct relationship was found between microstructure and magnetic properties.

Electron backscatter diffraction (EBSD) and electron probe microanalysis (EPMA) measurements are combined to characterize an industrial produced dual-phase steel containing some bainite fraction. High-resolution carbon mappings acquired on a field emission electron microprobe are utilized to validate and improve the identification of the constituents (ferrite, martensite, and bainite) performed by EBSD using the image quality and kernel average misorientation. The combination eliminates the ambiguity between the identification of bainite and transformation-induced dislocation zones, encountered if only the kernel average misorientation is considered. The detection of carbon in high misorientation regions confirms the presence of bainite. These results are corroborated by secondary electron images after nital etching. Limitations of this combined method due to differences between the spatial resolution of EBSD and EPMA are assessed. Moreover, a quantification procedure adapted to carbon analysis is presented and used to measure the carbon concentration in martensite and bainite on a submicrometer scale. From measurements on reference materials, this method gives an accuracy of 0.02 wt% C and a precision better than 0.05 wt% C despite unavoidable effects of hydrocarbon contamination.

Preparation of high-quality polished sample surfaces is an essential step in the collection of microanalytical data on the microstructures of minerals and alloys. Poorly prepared samples can yield insufficient or inconsistent results and, in the case of gold, potentially no data due to the “beilby” layer. Currently, preparation of ore samples is difficult as they commonly contain both hard and soft mineral phases. The aim of our research is to produce suitably polished sample surfaces, on all phases, for electron backscatter diffraction analysis. A combination of chemical–mechanical polishing (CMP) and broad ion-beam polishing (BIBP) was used to tackle the problem. Our results show that it is critical to perform CMP first, as it produces a suitable polish on the hard mineral phases but tends to introduce more damage to the soft mineral surfaces. BIBP is essential to produce a high-quality polish to the soft phases (gold). This is a highly efficient method of sample preparation and is important as it allows the complete quantification of ore textures and all constituent mineral phases, including soft alloys.

The influence on alloy 413.0 of the refinement and modification of its microstructure was analyzed by means of several microscopy techniques, as well as the effect of the application of high pressure during solidification. For each treatment and solidification pressure condition employed, the most suitable microscopy techniques for identifying and characterizing the phases present were investigated. Color metallography and electron microscopy techniques were applied to the qualitative microstructural analysis. Volume fraction and grain size of the primary α-Al were characterized by quantitative metallographic techniques. The results show that the effect caused by applying high pressure during solidification of the alloy is more pronounced than that caused by modification and refinement of the microstructure when it solidifies at atmospheric pressure. Furthermore, it has been shown that, for Al–Si alloy characterization, when aiming to characterize the primary α-Al phase, optical color metallography observed under crossed polarized light plus a sensitive tint filter is the most suitable technique. When the goal is to characterize the eutectic Si, the use of optical color metallography or electron microscopy is equally valid. The characterization of iron-rich intermetallic compounds should preferably be performed by means of backscattered electron imaging.

In situ scanning transmission electron microscopy (STEM) through liquids is a promising approach for exploring biological and materials processes. However, options for in situ chemical identification are limited: X-ray analysis is precluded because the liquid cell holder shadows the detector and electron energy-loss spectroscopy (EELS) is degraded by multiple scattering events in thick layers. Here, we explore the limits of EELS in the study of chemical reactions in their native environments in real time and on the nanometer scale. The determination of the local electron density, optical gap, and thickness of the liquid layer by valence EELS is demonstrated. By comparing theoretical and experimental plasmon energies, we find that liquids appear to follow the free-electron model that has been previously established for solids. Signals at energies below the optical gap and plasmon energy of the liquid provide a high signal-to-background ratio regime as demonstrated for LiFePO4 in an aqueous solution. The potential for the use of valence EELS to understand in situ STEM reactions is demonstrated for beam-induced deposition of metallic copper: as copper clusters grow, EELS develops low-loss peaks corresponding to metallic copper. From these techniques, in situ imaging and valence EELS offer insights into the local electronic structure of nanoparticles and chemical reactions.

Finding a faster alternative to tilt-series electron tomography is critical for rapidly evolving fields such as the semiconductor industry, where failure analysis could greatly benefit from higher throughput. We present a theoretical and experimental evaluation of scanning confocal electron energy-loss microscopy (SCEELM) using valence-loss signals, which is a promising technique for the reliable reconstruction of materials with sub-10-nm resolution. Such a confocal geometry transfers information from the focused portion of the electron beam and enables rapid three-dimensional (3D) reconstruction by depth sectioning. SCEELM can minimize or eliminate the missing-information cone and the elongation problem that are associated with other depth-sectioning image techniques in a transmission electron microscope. Valence-loss SCEELM data acquisition is an order of magnitude faster and requires little postprocessing compared with tilt-series electron tomography. With postspecimen chromatic aberration (Cc) correction, SCEELM signals can be acquired in parallel in the direction of energy dispersion with the aid of a physical pinhole. This increases the efficiency by 10×–100×, and can provide 3D resolved chemical information for multiple core-loss signals simultaneously.

The aberration-corrected scanning transmission electron microscope has great sensitivity to environmental or instrumental disturbances such as acoustic, mechanical, or electromagnetic interference. This interference can introduce distortions to the images recorded and degrade both signal noise and resolution performance. In addition, sample or stage drift can cause the images to appear warped and leads to unreliable lattice parameters being exhibited. Here a detailed study of the sources, natures, and effects of imaging distortions is presented, and from this analysis a piece of image reconstruction code has been developed that can restore the majority of the effects of these detrimental image distortions for atomic-resolution data. Example data are presented, and the performance of the restored images is compared quantitatively against the as-recorded data. An improvement in apparent resolution of 16% and an improvement in signal-to-noise ratio of 30% were achieved, as well as correction of the drift up to the precision to which it can be measured.

A new mathematical algorithm is reported for the accurate and efficient analysis of pore properties of nanoporous anodic alumina (NAA) membranes using scanning electron microscope (SEM) images. NAA membranes of the desired pore size were fabricated using a two-step anodic oxidation process. Surface morphology of the NAA membranes with different pore properties was studied using SEM images along with computerized image processing and analysis. The main objective was to analyze the SEM images of NAA membranes quantitatively, systematically, and quickly. The method uses a regularized shock filter for contrast enhancement, mathematical morphological operators, and a segmentation process for efficient determination of pore properties. The algorithm is executed using MATLAB, which generates a statistical report on the morphology of NAA membrane surfaces and performs accurate quantification of the parameters such as average pore-size distribution, porous area fraction, and average interpore distances. A good comparison between the pore property measurements was obtained using our algorithm and ImageJ software. This algorithm, with little manual intervention, is useful for optimizing the experimental process parameters during the fabrication of such nanostructures. Further, the algorithm is capable of analyzing SEM images of similar or asymmetrically porous nanostructures where sample and background have distinguishable contrast.

Quality control of the inertial confinement fusion (ICF) target in the laser fusion program is vital to ensure that energy deposition from the lasers results in uniform compression and minimization of Rayleigh–Taylor instabilities. The technique of nuclear microscopy with ion beam analysis is a powerful method to provide characterization of ICF targets. Distribution of elements, depth profile, and density image of ICF targets can be identified by particle-induced X-ray emission, Rutherford backscattering spectrometry, and scanning transmission ion microscopy. We present examples of ICF target characterization by nuclear microscopy at Fudan University in order to demonstrate their potential impact in assessing target fabrication processes.

Transmission electron microscopy (TEM) and focused ion beam (FIB) are proven tools to produce site-specific samples in which to study devices from initial processing to causes for failure, as well as investigating the quality, defects, interface layers, etc. However, the use of polymer substrates presents new challenges, in the preparation of suitable site-specific TEM samples, which include sample warping, heating, charging, and melting. In addition to current options that address some of these problems such as cryo FIB, we add an alternative method and FIB sample geometry that address these challenges and produce viable samples suitable for TEM elemental analysis. The key feature to this approach is a larger than usual lift-out block into which small viewing windows are thinned. Significant largely unthinned regions of the block are left between and at the base of the thinned windows. These large unthinned regions supply structural support and thermal reservoirs during the thinning process. As proof-of-concept of this sample preparation method, we also present TEM elemental analysis of various thin metallic films deposited on patterned polycarbonate, lacquer, and poly-di-methyl-siloxane substrates where the pattern (from low- to high-aspect ratio) is preserved.

Several problematic specimens, especially when composed of a complex three-dimensional architecture or very high or ultralow ranges in regional thickness and density, can be observed in improved clarity and precision when universal variable brightfield–darkfield contrast (UVBDC) is used. In this method, two different partial images are optically superimposed and interfere with each other, contributing to complementary visual information: a brightfield and a darkfield image. These images can be generated with concentric-peripheral, paraxial, or axial illuminating light. In all variants, variable transitions between bright- and darkfield are achievable. By use of a pancratic condenser (zoom system), the illuminating light can be universally adjusted and optimally adapted to each type of specimen and each type of objective (glass and mirror lenses). The concentric-peripheral variant is preferably carried out with normal glass lenses, the axial variant with mirror lenses. Glass lenses can also be used for UVBDC based on axial or paraxial light when combined with a special contrast tube, which is described in detail. Which technical variant of UVBDC might lead to the best result may be determined by the particular properties of the specimen, but all techniques described promise significant improvements in image quality and visual information.