Characterization of the topmost surface of biomaterials is crucial to understanding their properties and interactions with the local environment. In this study, the oxide layer microstructure of plasma-modified 316L stainless steel (SS316L) samples was analyzed by a combination of electron backscatter diffraction and electron channeling contrast imaging using low-energy incident electrons. Both techniques allowed clear identification of a nano-thick amorphous oxide layer, on top of the polycrystalline substrate, for the plasma-modified samples. A methodology was developed using Monte Carlo simulations combined with the experimental results to estimate thickness of the amorphous layer for different surface conditions. X-ray photoelectron spectroscopy depth profiles were used to validate these estimations.

The scanning electron microscope provides a platform for subnanometer resolution characterization of material morphology with excellent topographic and chemical contrast dependent on the used detectors. For imaging applications, the predominantly utilized signals are secondary electrons (SEs) and backscattered electrons (BSEs) that are emitted from the sample surface. Recent advances in detector technology beyond the traditional Everhart–Thornley geometry have enabled the simultaneous acquisition and discrimination of SE and BSE signals. This study demonstrates the imaging capabilities of a recently introduced new detector system that consists of the combination of two in-lens (I-L) detectors and one in-column (I-C) detector. Coupled with biasing the sample stage to reduce electron–specimen interaction volumes, this trinity of detector geometry allows simultaneous acquisition of signals to distinguish chemical contrast from topographical changes of the sample, including the identification of surface contamination. The I-C detector provides 4× improved topography, whereas the I-L detector closest to the sample offers excellent simultaneous chemical contrast imaging while not limiting the minimization of working distance to obtain optimal lateral resolution. Imaging capabilities and contrast mechanisms for all three detectors are discussed quantitatively in direct comparison to each other and the conventional Everhart–Thornley detector.

Abdominal aortic aneurysm is a multifactorial disease that is a leading cause of death in developed countries. Matrix-metalloproteases (MMPs) are part of the disease process, however, assessing their role in disease initiation and progression has been difficult and animal models have become essential. Combining Förster resonance energy transfer (FRET) proteolytic beacons activated in the presence of MMPs with 2-photon microscopy allows for a novel method of evaluating MMP activity within the extracellular matrix (ECM). Single and 2-photon spectra for proteolytic beacons were determined in vitro. Ex vivo experiments using the apolipoprotein E knockout angiotensin II-infused mouse model of aneurysm imaged ECM architecture simultaneously with the MMP-activated FRET beacons. 2-photon spectra of the two-color proteolytic beacons showed peaks for the individual fluorophores that enable imaging of MMP activity through proteolytic cleavage. Ex vivo imaging of the beacons within the ECM revealed both microstructure and MMP activity. 2-photon imaging of the beacons in aneurysmal tissue showed an increase in proteolytic cleavage within the ECM (p<0.001), thus indicating an increase in MMP activity. Our data suggest that FRET-based proteolytic beacons show promise in assessing MMP activity within the ECM and will therefore allow future studies to identify the heterogeneous distribution of simultaneous ECM remodeling and protease activity in aneurysmal disease.

A corrosion product rarely reported in the literature has been found on the copper support of three miniature paintings of the 17th and 18th centuries. This product, which has been identified as dicoppertrihydroxyformate (Cu2(OH)3HCOO), is an unusual basic copper formate found on copper artifacts. The identification and characterization of dicoppertrihydroxyformate was carried out directly over the corroded surface of the objects, using a nondestructive approach, which combines the integrated use of various microanalytical techniques. Using this approach, it was possible to obtain a set of new reference data about the natural form of Cu2(OH)3HCOO, that will enable its unambiguous identification in other similar objects. In this work, the probable causes that may have contributed to its formation are also discussed.

Carbon fibers exhibit exceptional properties such as high stiffness and specific strength, making them excellent reinforcements for composite materials. However, it is difficult to directly measure their tensile properties and estimates are often obtained by tensioning fiber bundles or composites. While these macro scale tests are informative for composite design, their results differ from that of direct testing of individual fibers. Furthermore, carbon filament strength also depends on other variables, including the test length, actual fiber diameter, and material flaw distribution. Single fiber tensile testing was performed on high-strength carbon fibers to determine the load and strain at failure. Scanning electron microscopy was also conducted to evaluate the fiber surface morphology and precisely measure each fiber’s diameter. Fiber strength was found to depend on the test gage length and in an effort to better understand the overall expected performance of these fibers at various lengths, statistical weak link scaling was performed. In addition, the true Young’s modulus was also determined by taking the system compliance into account. It was found that all properties (tensile strength, strain to failure, and Young’s modulus) matched very well with the manufacturers’ reported values at 20 mm gage lengths, but deviated significantly at other lengths.

Poly[sulfur-random-(1,3-diisopropenylbenzene)] copolymers synthesized via inverse vulcanization represent an emerging class of electrochemically active polymers recently used in cathodes for Li–S batteries, capable of realizing enhanced capacity retention (1,005 mAh/g at 100 cycles) and lifetimes of over 500 cycles. The composite cathodes are organized in complex hierarchical three-dimensional (3D) architectures, which contain several components and are challenging to understand and characterize using any single technique. Here, multimode analytical scanning and transmission electron microscopies and energy-dispersive X-ray/electron energy-loss spectroscopies coupled with multivariate statistical analysis and tomography were applied to explore origins of the cathode-enhanced capacity retention. The surface topography, morphology, bonding, and compositions of the cathodes created by combining sulfur copolymers with varying 1,3-diisopropenylbenzene content and conductive carbons have been investigated at multiple scales in relation to the electrochemical performance and physico-mechanical stability. We demonstrate that replacing the elemental sulfur with organosulfur copolymers improves the compositional homogeneity and compatibility between carbons and sulfur-containing domains down to sub-5 nm length scales resulting in (a) intimate wetting of nanocarbons by the copolymers at interfaces; (b) the creation of 3D percolation networks of conductive pathways involving graphitic-like outer shells of aggregated carbons; (c) concomitant improvements in the stability with preserved meso- and nanoscale porosities required for efficient charge transport.

Micro-scale observations in karst caves help to identify different processes that shaped local morphology. Scanning electron microscopy/energy-dispersive X-ray spectroscopy inspection of speleothems from two karst caves in Slovenia, Predjama and Črna Jama, confirmed the presence of sub-angular to sub-rounded detrital fragments of clay minerals, feldspars, quartz, Fe-oxides/hydroxides, rutile and Nb-rutile, xenotime, kassite, allanite, fluorapatite, epidote, ilmenite, monazite, sphene, and zircon, between 2 and 50 μm across. These occur in porous layers separating calcite laminae in the clayey coating on the layer below the surface of the speleothems, and are also incorporated within actual crystals. It is likely that they are derived from the weathered rocks of the Eocene flysch. Probably they were first transported into the caves by floodwaters forming cave sediments. Later, depending upon the climate conditions, they were moved by air currents or by water to the surface of active speleothems. They might also be redeposited from overlying soils enriched with wind-transported minerals from the flysch, or from higher passages filled with weathered flysch sediment, by drip water percolating through the fissured limestone. As some of the identified minerals are carriers of rare earth elements, Ti and Zr, their presence could affect any palaeoclimatic interpretations that are based upon the geochemical composition of the speleothems.

Resin composite materials that are used to restore tooth cervical lesions associated with gingival recessions can hamper healing after root coverage surgeries. This study evaluates the in vitro cytotoxic effect of five resin composites (two commercial and three experimental) on oral mesenchymal stem cells (MSCs) and the persistence of stemness properties in high passage MSCs. Sorption and solubility tests were made for all materials. MSCs were isolated from re-entry palatal and periodontal granulation tissues and were characterized and cultured on composite discs. Cytotoxicity of the materials was evaluated by the Alamar Blue viability test, by Paul Karl Horan (PKH) labeling, and by immunocytochemical staining for actin. Water and saliva sorption and solubility data revealed that two of the experimental materials behaved comparable with the marketed resin composites. The Alamar Blue viability test shows that both cell lines grew well on composite discs that seemed to induce no apparent toxic effects. No signs of disruption of cytoskeleton organization was seen. Experimental resin composites can be recommended for further investigation for obtaining approval for use. The standard minimal criteria were fulfilled for high passage MSCs. Palatal tissue regains its regenerative properties in terms of MSC presence in the re-entry area after 6 months of healing.

A systematic study has been carried out to compare the surface morphology, shell thickness, mechanical properties, and binding behavior of melamine–formaldehyde microcapsules of 5–30 μm diameter size with various amounts of core content by using scanning and transmission electron microscopy including electron tomography, in situ nanomechanical tensile testing, and electron energy-loss spectroscopy. It is found that porosities are present on the outside surface of the capsule shell, but not on the inner surface of the shell. Nanomechanical tensile tests on the capsule shells reveal that Young’s modulus of the shell material is higher than that of bulk melamine–formaldehyde and that the shells exhibit a larger fracture strain compared with the bulk. Core-loss elemental analysis of microcapsules embedded in epoxy indicates that during the curing process, the microcapsule-matrix interface remains uniform and the epoxy matrix penetrates into the surface micro-porosities of the capsule shells.

Fluorescence-detected linear dichroism (FDLD) microscopy provides observation of structural order in a microscopic sample and its expression in numerical terms, enabling both quantitative and qualitative comparison among different samples. We applied FDLD microscopy to compare the distribution and alignment of cellulose fibrils in cell walls of compression wood (CW) and normal wood (NW) on stem cross-sections of juvenile Picea omorika trees. Our data indicate a decrease in cellulose fibril order in CW compared with NW. Radial and tangential walls differ considerably in both NW and CW. In radial walls, cellulose fibril order shows a gradual decrease from NW to severe CW, in line with the increase in CW severity. This indicates that FDLD analysis of cellulose fibril order in radial cell walls is a valuable method for estimation of CW severity.

The damage and ion distribution induced in Si by an inductively coupled plasma Xe focused ion beam was investigated by atom probe tomography. By using predefined patterns it was possible to prepare the atom probe tips with a sub 50 nm end radius in the ion beam microscope. The atom probe reconstruction shows good agreement with simulated implantation profiles and interplanar distances extracted from spatial distribution maps. The elemental profiles of O and C indicate co-implantation during the milling process. The presence of small disc-shaped Xe clusters are also found in the three-dimensional reconstruction. These are attributed to the presence of Xe nanocrystals or bubbles that open during the evaporation process. The expected accumulated dose points to a loss of >95% of the Xe during analysis, which escapes undetected.

In this study, an integrated analytical method was developed to investigate the composition of both the inorganic pigments and organic binders of polychrome relics in Maiji Mountain Grottoes in northwestern China. Cross-sections of each sample were prepared at the beginning of the study, and all experiments were carried out on these cross-sections. Polychromic structures were revealed by optical microscopy and scanning electron microscopy-backscattered electron imaging. Inorganic materials were determined by using SEM coupled with an energy dispersive spectrometer and μ-Raman spectrometer, whereas organic materials were identified by staining techniques and highly sensitive and specific immunofluorescence microscopy. Data showed that the red colors are attributed to one or two pigments of red ochre, cinnabar, and minium; the blue pigment is natural lazurite; the green pigment is ascribed to atacamite; the white color is attributed to potassium feldspar; and the black surface is formed by the discoloration of minium to plattnerite under the influence of environmental factors. Regarding organic binders used in painting and preparation layers, mammalian animal glue and chicken egg white were both found alone or in mixture. Finally, the conclusion is made that the Secco technique is employed in polychrome relics from Maiji Mountain Grottoes.

Phase identification of multi-phase materials provides essential information relating the material to its mechanical properties. In this study we selected DP980, a type of dual-phase steel, to investigate the content of martensite and ferrite grains. A combination of advanced techniques was used to provide detailed and precise information of the microstructure. Scanning and transmission electron microscopy were used to provide observations of the sample surface at different scales. Martensite and ferrite phases of DP980 were further identified and characterized using electron backscatter diffraction and scanning probe microscopy. Results obtained with nanoindentation tests confirmed that the differences in nanohardness values in single-phase grains are martensite and ferrite with different surface heights shown by scanning probe microscopy. The similarity shown in the image quality map and scanning probe microscopy proves that a large fraction of martensite can be distinguished in this undeformed material using image quality parameters obtained during electron backscatter diffraction imaging.

We report electron probe microanalysis measurements on nickel silicides, Ni5Si2, Ni2Si, Ni3Si2, and NiSi, which were done in order to investigate anomalies that affect the analysis of such materials by using the Ni L3-M4,5 line (Lα). Possible sources of systematic discrepancies between experimental data and theoretical predictions of Ni L3-M4,5k-ratios are examined, and special attention is paid to dependence of the Ni L3-M4,5k-ratios on mass-attenuation coefficients and partial fluorescence yields. Self-absorption X-ray spectra and empirical mass-attenuation coefficients were obtained for the considered materials from X-ray emission spectra and relative X-ray intensity measurements, respectively. It is shown that calculated k-ratios with empirical mass attenuation coefficients and modified partial fluorescence yields give better agreement with experimental data, except at very low accelerating voltages. Alternatively, satisfactory agreement is also achieved by using the Ni L3-M1 line (Lℓ) instead of the Ni L3-M4,5 line.