Several authors have reported the workability, mechanical properties, and durability of concrete produced with construction waste replacing the natural aggregate. However, a systematic microstructural characterization of recycled aggregate concrete has not been reported. This work studies the use of fine recycled aggregate to replace fine natural aggregate in the production of concrete and reports the resulting microstructures. The used raw materials were natural aggregate, recycled aggregate obtained from a standard concrete, and Portland cement. The substitution extent was 0, 10, 50, and 100 vol%; hydration was stopped at 9, 24, and 96 h and 28 days. Microscopy was focused on the cement/aggregate interfacial transition zone, enlightening the effect of incorporating recycled aggregate on the formation and morphology of the different concrete hydration products. The results show that concretes with recycled aggregates exhibit typical microstructural features of the transition zone in normal strength concrete. Although overall porosity increases with increasing replacement, the interfacial bond is apparently stronger when recycled aggregates are used. An addition of 10 vol% results in a decrease in porosity at the interface with a corresponding increase of the material hardness. This provides an opportunity for development of increased strength Portland cement concretes using controlled amounts of concrete waste.

Copper, gold, and tungsten thin films have been exposed to 30 kV Ga+ ion irradiation, and the resulting microstructural modifications are studied as a function of ion dose. The observed microstructural changes include texture development with respect to the easy channeling direction in the target, and in the case of Cu, an additional intermetallic phase is produced. Texture development in these target materials is a function of the starting materials grain size, and these changes are not observed in large grained materials. The accepted models of differential damage driven grain growth are not supported by the results of this study. The implications of this study to the use of focused ion beam tools for sample preparation are discussed.

Lithium sulfur (Li–S) batteries have the potential to provide higher energy storage density at lower cost than conventional lithium ion batteries. A key challenge for Li–S batteries is the loss of sulfur to the electrolyte during cycling. This loss can be mitigated by sequestering the sulfur in nanostructured carbon–sulfur composites. The nanoscale characterization of the sulfur distribution within these complex nanostructured electrodes is normally performed by electron microscopy, but sulfur sublimates and redistributes in the high-vacuum conditions of conventional electron microscopes. The resulting sublimation artifacts render characterization of sulfur in conventional electron microscopes problematic and unreliable. Here, we demonstrate two techniques, cryogenic transmission electron microscopy (cryo-TEM) and scanning electron microscopy in air (airSEM), that enable the reliable characterization of sulfur across multiple length scales by suppressing sulfur sublimation. We use cryo-TEM and airSEM to examine carbon–sulfur composites synthesized for use as Li–S battery cathodes, noting several cases where the commonly employed sulfur melt infusion method is highly inefficient at infiltrating sulfur into porous carbon hosts.

Interactions between cells and the surrounding extracellular matrix are important for a number of developmental events. In the heart, cardiac fibroblasts produce the majority of extracellular matrix proteins, particularly collagen types I and III. Cells originating from the proepicardial organ migrate over the surface of the heart, invade the underlying myocardium and ultimately give rise to smooth muscle cells, fibroblasts, and coronary endothelium. Although integrin expression in the developing heart has been well characterized, the expression of Discoidin Domain Receptor 2 (DDR2) remains to be defined. Using confocal microscopy, the expression of DDR2 was examined at several points during cardiac development. Initially, DDR2 expression was detected on the epicardial surface of the heart and on endothelial and mesenchymal cells within the cardiac cushions. As development progressed, DDR2 expression increased at localized regions in the apex and atrioventricular sulcus, although this expression decreased from epicardial to endocardial surface. Eventually, DDR2 expression spanned the myocardial free wall and was detected within the septum. Not until postnatal development was DDR2 expression detected uniformly throughout the myocardium and this distribution was maintained in the adult heart. In summary, the data presented demonstrate that the distribution of DDR2-positive cells changes within the heart during development.

The application of scanning electron microscopy (SEM) and secondary ion mass spectrometry (SIMS) for characterization of mixed plutonium and uranium particles from nuclear weapons material is presented. The particles originated from the so-called Thule accident in Greenland in 1968. Morphological properties have been studied by SEM and two groups were identified: a “popcorn” structure and a spongy structure. The same technique, coupled with an energy-dispersive X-ray (EDX) spectrometer, showed a heterogeneous composition of Pu and U in the surface layers of the particles. The SIMS depth profiles revealed a varying isotopic composition indicating a heterogeneous mixture of Pu and U in the original nuclear weapons material itself. The depth distributions agree with synchrotron-radiation-based μ-XRF (X-ray fluorescence microprobe) measurements on the particle (Eriksson, M., Wegryzynek, D., Simon, R., & Chinea-Cano, E., in prep.) when a SIMS relative sensitivity factor for Pu to U of 6 is assumed. Different SIMS identified isotopic ratio groups are presented, and the influence of interferences in the Pu and U mass range are estimated. The study found that the materials are a mixture of highly enriched 235U (235U:238U ratio from 0.96 to 1.4) and so-called weapons grade Pu (240Pu:239Pu ratio from 0.028 to 0.059) and confirms earlier work reported in the literature.

The article presents a review of the use of cross-section and staining techniques for investigating natural organic materials (mainly proteinaceous and oil-based binders/varnishes) in painted and polychrome artworks, considering the requirements of conservation practice and routine diagnostics. The reviewed literature calls attention to the importance of using cross sections to prepare samples for optical microscopy and to different properties of embedding resins; the most appropriate instrumental conditions for optical microscopy; and the advantages and disadvantages of the most common staining techniques. A few case studies were selected to illustrate the use of autofluorescence (intrinsic fluorescence) and induced fluorescence (using specific staining tests and fluorophore-labeled antibodies) for mapping and identifying organic paint materials in cross sections. New directions of research in cross-section analyses and fluorescence-based techniques for the identification and mapping of artistic materials are presented. The complementary use of different stains on the same cross section, further exploration of intrinsic and induced fluorescence of aged versus fresh materials, and applicability of cross-section observation and staining as complementary methods for assessing the effectiveness of restoration treatments, such as cleaning and consolidation, are discussed in the last section of the article.

The recent development of in-situ liquid stages for (scanning) transmission electron microscopes now makes it possible for us to study the details of electrochemical processes under operando conditions. As electrochemical processes are complex, care must be taken to calibrate the system before any in-situ/operando observations. In addition, as the electron beam can cause effects that look similar to electrochemical processes at the electrolyte/electrode interface, an understanding of the role of the electron beam in modifying the operando observations must also be understood. In this paper we describe the design, assembly, and operation of an in-situ electrochemical cell, paying particular attention to the method for controlling and quantifying the experimental parameters. The use of this system is then demonstrated for the lithiation/delithiation of silicon nanowires.

Diabetes is an increasing public health problem that is expected to escalate in the future due to the growing incidence of obesity in the western world. While this disease is well known for its devastating effects on the kidneys and vascular system, diabetic individuals can develop cardiac dysfunction, termed diabetic cardiomyopathy, in the absence of other cardiovascular risk factors such as hypertension or atherosclerosis. While much effort has gone into understanding the effects of elevated glucose or altered insulin sensitivity on cellular components within the heart, significant changes in the cardiac extracellular matrix (ECM) have also been noted. In this review article we highlight what is currently known regarding the effects diabetes has on both the expression and chemical modification of proteins within the ECM and how the fibrotic response often observed as a consequence of this disease can contribute to reduced cardiac function.

The present study planned to assess the medicinally important plants in the lower Margalla Hills of Islamabad, Pakistan using scanning electron microscopy of their pollens. Both quantitative and qualitative characters of the pollens were analyzed. The shapes of the pollen were prolate, spheroidal, elliptical, and oblate. Exine sculpturing showed rugulate, scabrate, psilate gemmate, and reticulate ornamentation. The people residing in the rural areas are thought to depend, primarily, on medicinal plant resources for many health care needs. A sample of 140 respondents was selected and interviewed by using a stratified random sampling technique. Results showed that the local communities of lower Margalla Hills are highly dependent on plants to treat various ailments, for example, respiratory (28%), digestive (46%) nervous, circulatory and dermatological problems (6% each), and reproductive problems (8%). The continuous dependence of the local community on ethnomedicinally important plants has led to serious degradation of the natural forest of lower Margalla Hills. Priority-based conservation and sustainable use of these forest resources are necessary, and use of alternative resources will also help in the forest conservation.

XFILM is a computer program for determining the thickness and composition of thin films on substrates and multilayers by electron probe microanalysis. In this study, we describe the X-ray emission model implemented in the latest version of XFILM and assess its reliability by comparing measured and calculated k-ratios from thin-film samples available in the literature. We present and discuss examples of applications of XFILM that illustrate the capabilities of the program.

Aberration-corrected scanning transmission electron microscopes (STEMs) provide sub-Angstrom lateral resolution; however, the large convergence angle greatly reduces the depth of field. For microscopes with a small depth of field, information outside of the focal plane quickly becomes blurred and less defined. It may not be possible to image some samples entirely in focus. Extended depth-of-field techniques, however, allow a single image, with all areas in focus, to be extracted from a series of images focused at a range of depths. In recent years, a variety of algorithmic approaches have been employed for bright-field optical microscopy. Here, we demonstrate that some established optical microscopy methods can also be applied to extend the ∼6 nm depth of focus of a 100 kV 5th-order aberration-corrected STEM (αmax = 33 mrad) to image Pt-Co nanoparticles on a thick vulcanized carbon support. These techniques allow us to automatically obtain a single image with all the particles in focus as well as a complimentary topography map.

Irradiation of reactor pressure vessel (RPV) steels causes the formation of nanoscale microstructural features (termed radiation damage), which affect the mechanical properties of the vessel. A key tool for characterizing these nanoscale features is atom probe tomography (APT), due to its high spatial resolution and the ability to identify different chemical species in three dimensions. Microstructural observations using APT can underpin development of a mechanistic understanding of defect formation. However, with atom probe analyses there are currently multiple methods for analyzing the data. This can result in inconsistencies between results obtained from different researchers and unnecessary scatter when combining data from multiple sources. This makes interpretation of results more complex and calibration of radiation damage models challenging. In this work simulations of a range of different microstructures are used to directly compare different cluster analysis algorithms and identify their strengths and weaknesses.

Stereological analysis has been coupled with transmission electron microscope (TEM) orientation mapping to investigate the grain boundary character distribution in nanocrystalline copper thin films. The use of the nanosized (<5 nm) beam in the TEM for collecting spot diffraction patterns renders an order of magnitude improvement in spatial resolution compared to the analysis of electron backscatter diffraction patterns in the scanning electron microscope. Electron beam precession is used to reduce dynamical effects and increase the reliability of orientation solutions. The misorientation distribution function shows a strong misorientation texture with a peak at 60°/[111], corresponding to the Σ3 misorientation. The grain boundary plane distribution shows {111} as the most frequently occurring plane, indicating a significant population of coherent twin boundaries. This study demonstrates the use of nanoscale orientation mapping in the TEM to quantify the five-parameter grain boundary distribution in nanocrystalline materials.

With the availability of resolution boosting and delocalization minimizing techniques, for example, spherical aberration correction and exit-plane wave function reconstruction, high-resolution transmission electron microscopy is drawing to a breakthrough with respect to the atomic-scale imaging of common semiconductor materials. In the present study, we apply a combination of these two state-of-the-art techniques to investigate lattice defects in GaAs-based heterostructures at atomic resolution. Focusing on the direct imaging of stacking faults as well as the core structure of edge and partial dislocations, the practical capabilities of both techniques are illustrated. For the first time, we apply the technique of bright-atom contrast imaging at negative spherical aberration together with an appropriate overfocus setting for the investigation of lattice defects in a semiconductor material. For these purposes, the elastic displacements associated with lattice defects in GaAs viewed along the [110] zone axis are measured from experimental images using reciprocal space strain map algorithms. Moreover, we demonstrate the benefits of the retrieval of the exit-plane wave function not only for the elimination of residual imaging artefacts but also for the proper on-line alignment of specimens during operation of the electron microscope—a basic prerequisite to obtain a fair agreement between simulated images and experimental micrographs.

Here, we report the development of an approach to map atomic resolution images into a convenient matrix representation. Through the combination of two-dimensional Gaussian fitting and the projective standard deviation, atom column locations are projected onto two noncollinear reference lattice vectors that are used to assign each a unique (i, j) matrix index. By doing so, straightforward atomic resolution image analysis becomes possible. Using practical examples, we demonstrate that the matrix representation greatly simplifies categorizing atom columns to different sublattices. This enables a myriad of direct analyses, such as mapping atom column properties and correlating long-range atom column pairs. MATLAB source code can be downloaded from https://github.com/subangstrom/aci.

A calibration procedure for the detection efficiency of energy dispersive X-ray spectrometers (EDS) used in combination with scanning electron microscopy (SEM) for standardless electron probe microanalysis (EPMA) is presented. The procedure is based on the comparison of X-ray spectra from a reference material (RM) measured with the EDS to be calibrated and a reference EDS. The RM is certified by the line intensities in the X-ray spectrum recorded with a reference EDS and by its composition. The calibration of the reference EDS is performed using synchrotron radiation at the radiometry laboratory of the Physikalisch-Technische Bundesanstalt. Measurement of RM spectra and comparison of the specified line intensities enables a rapid efficiency calibration on most SEMs. The article reports on studies to prepare such a RM and on EDS calibration and proposes a methodology that could be implemented in current spectrometer software to enable the calibration with a minimum of operator assistance.

The composition of co-precipitated and collocated NbC carbide precipitates, Fe3C iron carbide (cementite), and Cu-rich precipitates are studied experimentally by atom-probe tomography (APT). The Cu-rich precipitates located at a grain boundary (GB) are also studied. The APT results for the carbides are supplemented with computational thermodynamics predictions of composition at thermodynamic equilibrium. Two types of NbC carbide precipitates are distinguished based on their stoichiometric ratio and size. The Cu-rich precipitates at the periphery of the iron carbide and at the GB are larger than those distributed in the α-Fe (body-centered cubic) matrix, which is attributed to short-circuit diffusion of Cu along the GB. Manganese segregation is not observed at the heterophase interfaces of the Cu-rich precipitates that are located at the periphery of the iron carbide or at the GB, which is unlike those located at the edge of the NbC carbide precipitates or distributed in the α-Fe matrix. This suggests the presence of two populations of NiAl-type (B2 structure) phases at the heterophase interfaces in multicomponent Fe–Cu steels.

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.