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Summary: This paper takes a fundamental view of the electron energy loss spectra of monolayer and few layer MoS2. The dielectric function of monolayer MoS2 is compared to the experimental spectra to give clear criteria for the nature of different signals. Kramers–Krönig analysis allows a direct extraction of the dielectric function from the experimental data. However this analysis is sensitive to slight changes in the normalisation step of the data pretreatment. Density functional theory provides simulations of the dielectric function for comparison and validation of experimental findings. Simulated and experimental spectra are compared to isolate the π and π + σ surface plasmon modes in monolayer MoS2. Single‐particle excitations obscure the plasmons in the monolayer spectrum and momentum resolved measurements give indication of indirect interband transitions that are excited due to the large convergence and collection angles used in the experiment. Lay Description: Two‐dimensional materials offer a path forward for smaller and more efficient devices. Their optical and electronic properties give way to beat the limits set in place by Moore's Law. Plasmon are the collective oscillations of electrons and can confine light to dimensions much smaller than its wavelength. In this work we explore the plasmonic properties of MoS2, a representational candidate from a family of 2D materials known as transition metal dichalcogenides. High resolution electron microscopy and spectroscopy provide insights in the plasmonic properties of MoS2 down to an atomic scale. Experimental results show the relationship between plasmons and interband transitions in the electron energy loss spectrum. Density functional theory provides a theoretical support for the experimental findings and provides commentary on the fundamental underlying physics. [ABSTRACT FROM AUTHOR]

Summary: Regeneration of diesel particulate filter (DPF) is a complicated process due to its high operating temperature and associated oxidation of soot on the filter substrate. Several oxidation mechanisms of diesel soot have been proposed based on reaction kinetics, but more information about the oxidation phenomena is needed in a practical system, that is, soot oxidation on a DPF substrate. In this work, the DPF regeneration process was, for the first time, visualized at the particle scale ex‐situ, in time‐lapse series, using field emission scanning electron microscopy (FE‐SEM). Time‐lapse transformation of soot cake layer on a real DPF was followed from initiation through the complete regeneration process. In parallel, transformation of the soot primary particle diameter was directly measured using high‐resolution transmission electron microscopy. FE‐SEM visualization clearly showed shrinkage of the soot cake layer on the DPF wall as oxidation progressed. Furthermore, diameter distribution analysis revealed a trend of shrinkage of the nanoscale soot primary particles during oxidation, supporting the FE‐SEM observations of the micron‐scale shrinkage of the agglomerated soot cake layer. Fragmentation of the shrunken soot cake layer was also observed and is suspected to be a result of locally higher gas flow that depends on surface pore morphology of the filter substrate. Lay Description: In this work, the DPF regeneration process was, for the first time, visualized at the particle scale ex‐situ, in time‐lapse series, using field emission scanning electron microscopy (FE‐SEM). Time‐lapse transformation of soot cake layer on a real DPF was followed from initiation through the complete regeneration process. In parallel, transformation of the soot primary particle diameter was directly measured using high resolution transmission electron microscopy. FE‐SEM visualization clearly showed shrinkage of the soot cake layer on the DPF wall as oxidation progressed. Furthermore, diameter distribution analysis revealed a trend of shrinkage of the nano‐scaled soot primary particles during oxidation, supporting the FE‐SEM observations of the shrinkage of the micron‐scale agglomerated soot cake layer. Fragmentation of the shrunken soot cake layer was also observed and is suspected to be a result of locally higher gas flow that depends on surface pore morphology of the filter substrate. Further detail mechanism about transformations of the soot cake layer was additionally discussed based on electrostatic attraction. [ABSTRACT FROM AUTHOR]

Summary: Geometrical phase analysis (GPA) is typically a powerful tool to investigate the deformation in high resolution transmission electron microscopy images and has been used in various fields. During GPA, strain components are calculated relative to an undistorted reference region. In the present work, the effect of reference region size on strain measurements has been investigated. Experimental measurements on a locally distorted gold nanoparticle exhibited that a small reference region below the GPA spatial resolution can introduce an inaccuracy in the measured displacement field, which appears as a significant increase in measured strains and severe fluctuation in phase images. The inaccuracy may be ascribed to an error of insufficient sampling. Our results suggest that a small reference region below the GPA spatial resolution should be avoided during GPA. This prerequisite should be paid more attention to during strain measurement on nanoparticles. [ABSTRACT FROM AUTHOR]

Manipulation of viable Yersinia pestis (etiologic agent of plague) in the laboratory usually necessitates elevated biosafety and biocontainment procedures, even with avirulent or vaccine strains. To facilitate downstream biochemical or physical analyses in a Biosafety Level 1 laboratory environment, effective inactivation without affecting its intrinsic properties is critical. Here, we report on the morphological and biochemical changes to Y. pestis surfaces following four different fixation methods that render the cells nonviable. The results, obtained at the single cell level, demonstrate that methanol inactivation is best able to preserve bacterial morphology and bioactivity, enabling subsequent analysis. This nanoscale evaluation of the effects of inactivation on cell morphology and surface bioactivity may provide a crucial preparatory approach to study virulent pathogens in the lab setting using high-resolution microscopic techniques such as atomic force microscopy. [ABSTRACT FROM AUTHOR]

Precipitates and solute enrich in aged ferritic steel containing copper were examined using high-resolution electron microscopy, high-angle annular dark-field scanning transmission electron microscopy and energy-dispersive X-ray spectroscopy. Two ledgeswith one-atom and two-atom layers height in the 9R/3R interface were observed. The enrichment of copper into two successive closed-packed planes with an interval of Fe-rich close-packed plane was detected. The passage of the Shockley partial, or the shearing, changes the stacking sequence of closed-packed planes. Finally, 9R Cu variant transformed into 3R Cu variant. [ABSTRACT FROM AUTHOR]

Continuous research on small-scale mechanical structures and systems has attracted strong demand for ultrafine deformation and strain measurements. Conventional optical microscope cannot meet such requirements owing to its lower spatial resolution. Therefore, high-resolution scanning electronmicroscope has become the preferred system for high spatial resolution imaging and measurements. However, scanning electron microscope usually is contaminated by distortion and drift aberrations which cause serious errors to precise imaging and measurements of tiny structures. This paper develops a new method to correct drift and distortion aberrations of scanning electron microscope images, and evaluates the effect of correction by comparing corrected images with scanning electron microscope image of a standard sample. The drift correction is based on the interpolation scheme, where a series of images are captured at one location of the sample and perform image correlation between the first image and the consequent images to interpolate the drift-time relationship of scanning electron microscope images. The distortion correction employs the axial symmetry model of charged particle imaging theory to two images sharing with the same location of one object under different imaging fields of view. The difference apart from rigid displacement between the mentioned two images will give distortion parameters. Three-order precision is considered in the model and experiment shows that one pixel maximum correction is obtained for the employed high-resolution electronmicroscopic system. [ABSTRACT FROM AUTHOR]

Cross-sectional transmission electron microscopy and X-ray phase analysis were used to study the structure of a layer formed during nitriding the AISI 316L stainless steel at temperature 440°C. It was found that the applied treatment led to the formation of 6-μm-thick layer of the S-phase. There is no evidence of CrN precipitation. The X-ray diffraction experiments proved that the occurred austenite lattice expansion – due to nitrogen atoms – depended on the crystallographic direction. The cross-sectional transmission electron microscopy studies showed that the layer consisted of a single cubic phase that contained a lot of defects such as dislocations, stacking faults, slip bands and twins. The high-resolution electron microscopy observations were applied to study the defect formation due to the nitriding process. It was shown that the presence of great number of stacking faults leads to formation of nanotwins. Weak, forbidden {100} reflections were still another characteristic feature of the S-phase. These were not detected in the X-ray spectra of the phase. Basing on the high-resolution electron microscopy studies it can be suggested that the short-range ordering of the nitrogen atoms in the octahedral sites inside the f.c.c. matrix lattice takes place and gives rise to appearance of these spots. It is suggested that the cubic lattice undergoes not only expansion but also slight rombohedral distortion that explains differences in the lattice expansion for different crystallographic directions. [ABSTRACT FROM AUTHOR]

The zirconia nanopowder stabilized with 2.5 mol% Y2O3 and doped with 18 mol% TiO2 (Zr(Y,Ti)O2) was homogenized with 5.2 wt% multiwall carbon nanotubes (MWCNT) through colloidal processing. The resultant mixture was heat-treated for 2 h at 1200°C in vacuum under a pressure of 5 · 10−4 mbar. The microstructure characterization was performed using the TECNAI FEG (200 kV) SuperTWIN transmission electron microscope, equipped with the integrated EDAX detector. The TEM observations of the as-received samples showed single strands of the carbon nanotubes uniformly dispersed among zirconia crystallites. Heat treatment of the Zr(Y,Ti)O2-MWCNT mixture caused the transformation of carbon nanotubes into polycrystalline TiC nanofibres and nanorods as confirmed by both the energy dispersive X-ray spectroscopy microanalysis and the high-resolution electron microscopy (HREM) observations. Relying on the above, a mechanism of the TiC in situ crystallization controlled by carbon diffusion through the newly formed TiC phase was discussed. [ABSTRACT FROM AUTHOR]

Nanocomposites consisting of one-dimensional CuI crystals inside single-walled carbon nanotubes were obtained using the capillary technique. high-resolution transmission electron microscopy investigations of the atomic structure of the encapsulated 1D CuI crystals revealed two types of 1D CuI crystals with growth direction <001> and relative to the bulk hexagonal CuI structure. Atomic structure models were proposed based on the high-resolution transmission electron microscopy images. According to the proposed models and image simulations, the main contrast in the 1D crystal images arises from the iodine atoms whereas copper atoms, with lower atomic number giving lower contrast, are thought to be statistically distributed. [ABSTRACT FROM AUTHOR]

The zirconia nanopowder stabilized with 2.5 mol% Y2O3 and doped with 18 mol% TiO2 (Zr(Y,Ti)O2) was homogenized with 5.2 wt% multiwall carbon nanotubes (MWCNT) through colloidal processing. The resultant mixture was heat-treated for 2 h at 1200°C in vacuum under a pressure of 5 · 10−4 mbar. The microstructure characterization was performed using the TECNAI FEG (200 kV) SuperTWIN transmission electron microscope, equipped with the integrated EDAX detector. The TEM observations of the as-received samples showed single strands of the carbon nanotubes uniformly dispersed among zirconia crystallites. Heat treatment of the Zr(Y,Ti)O2-MWCNT mixture caused the transformation of carbon nanotubes into polycrystalline TiC nanofibres and nanorods as confirmed by both the energy dispersive X-ray spectroscopy microanalysis and the high-resolution electron microscopy (HREM) observations. Relying on the above, a mechanism of the TiC in situ crystallization controlled by carbon diffusion through the newly formed TiC phase was discussed. [ABSTRACT FROM AUTHOR]

Peak-finding procedures and the geometric phase method of quantitative high resolution electron microscopy (qHRTEM) were applied to determine the local strain and the chemical composition of nanostructured semiconductor materials. The growth of the structures investigated was induced by minimization of strain energy. The analysis of strain distribution is necessary for the understanding of the self-organized formation of nanostructures. The possibilities and limitations of the methods are discussed in detail by analysing HRTEM images of (Si,Ge) islands and of a double layer of stacked quantum dots of (In,Ga)As and Ga(Sb,As). [ABSTRACT FROM AUTHOR]

High Resolution Electron Microscopy (HREM) is often used to characterize objects supported by amorphous substrates, usually amorphous carbon. HREM is currently undergoing step change in performance due to aberration correctors. This paper examines the aberration corrected imaging of objects supported by amorphous substrates. In particular, we show that a substantial increase in the ratio of the object contrast to the substrate contrast can be achieved by utilizing the strong variation of phase contrast with height, which is present when the spherical aberration has been adjusted to a small value. This variation is examined using the familiar Weak Phase Object Approximation model from which it is determined that the contrast ratio achieves a maximum at a small nonzero value of the spherical aberration. This result is confirmed by multislice modelling which allows for deviations from the Weak Phase Object Approximation and delocalization effects. One important practical result of this study is the need to place the object of interest on the correct side of the amorphous carbon substrate. [ABSTRACT FROM AUTHOR]

The decreasing process of oxygen in YBa2Cu3Oy is investigated through high resolution electron microscopy (HREM) and convergent beam electron diffraction (CBED). Measurements of the axial length in HREM images show that oxygen content y decreases faster near a twin boundary than at the inner part of a twin lamella. The transformation from an orthorhombic to a tetragonal phase starts at a twin boundary and the transformed region propagates to an inner region of lamella. Lattice strains are observed near boundaries between transformed and non-transformed regions. The transformation is almost complete within 30 s during observation of HREM images at 400 kV and at room temperature. A value of y was quantitatively measured by analysing observed intensities of energy-filtered CBED patterns with the dynamical theory. The value of y decreases from 6.9 to 6.5 when 200 kV electrons are irradiated for 160 s in a microscope at 108 K. More precise analysis of the intensities provides information on charge distribution along the c-axis as well as local oxygen content at a spatial resolution of several nanometres. [ABSTRACT FROM AUTHOR]

The decreasing process of oxygen in YBa2Cu3Oy is investigated through high resolution electron microscopy (HREM) and convergent beam electron diffraction (CBED). Measurements of the axial length in HREM images show that oxygen content y decreases faster near a twin boundary than at the inner part of a twin lamella. The transformation from an orthorhombic to a tetragonal phase starts at a twin boundary and the transformed region propagates to an inner region of lamella. Lattice strains are observed near boundaries between transformed and non-transformed regions. The transformation is almost complete within 30 s during observation of HREM images at 400 kV and at room temperature. A value of y was quantitatively measured by analysing observed intensities of energy-filtered CBED patterns with the dynamical theory. The value of y decreases from 6.9 to 6.5 when 200 kV electrons are irradiated for 160 s in a microscope at 108 K. More precise analysis of the intensities provides information on charge distribution along the c-axis as well as local oxygen content at a spatial resolution of several nanometres. [ABSTRACT FROM AUTHOR]

The structure of Al3Zr precipitates in Al-1.0Mg-0.6Si-0.5Zr (in wt.%) alloy was investigated using conventional transmission electron microscopy (TEM) and high-resolution TEM (HREM). After annealing of the alloy in the temperature range 450–540 °C, spherical precipitates of metastable L12-Al3Zr phase appeared nearly homogeneously within the matrix, and elongated particles were found at grain boundaries. L12-structured Al3Zr were about 20–30 nm in diameter and coherent with the matrix. Inside some of them, planar faults parallel to {100} planes were revealed by use of HREM. Most probably, these faults are an indication of the transition stage of transformation to the stable D023-type Al3Zr phase. The elongated precipitates (about 100 nm) were identified as D022-type Al3Zr. Energy-dispersive X-ray analysis showed that they contain, apart from Al, mainly Zr with small amounts of Si. The substitution of Al by Si increased the stability of the D022-Al3Zr as compared with D023-Al3Zr. [ABSTRACT FROM AUTHOR]

In a boron nitride thin film, grown on a Si (100) substrate by radio frequency magnetron sputtering, a striking nanostructure is observed by high-resolution transmission electron microscopy. It consists of cubic boron nitride nanocrystals with a rather good triangular shape, pointing always to the substrate. The nanocrystals are usually highly defected and present their own interesting internal structure. Texture formation is observed within a nanocrystal, with all the subgrains observed to have a common <011> axis, which is also approximately parallel to a <011> axis of the Si substrate, i.e. the nanocrystals are very well structurally orientated in relation to the Si substrate (self-organized). Dislocations and stacking faults are also found in the nanocrystals. [ABSTRACT FROM AUTHOR]