Traditional electron microscopy techniques such as bright-field imaging provide poor contrast for organic films and identification of structures in amorphous material can be problematic, particularly in high-performance organic solar cells. By combining energy-filtered corrected transmission electron microscopy, together with electron energy loss and X-ray energy-dispersive hyperspectral imaging, we have imaged PTB7/PC61BM blended polymer optical photovoltaic films, and were able to identify domains ranging in size from several hundred nanometers to several nanometers in extent. This work verifies that microstructural domains exist in bulk heterojunctions in PTB7/PC61BM polymeric solar cells at multiple length scales and expands our understanding of optimal device performance providing insight for the design of even higher performance cells.

In this paper we investigate methods to characterize angular current density from atomically defined gas field ion sources. We show that the ion beam emitted from a single apex atom is described by a two-dimensional Gaussian profile. Owing to the Gaussian shape of the beam and the requirement to collect the majority of the ion current, fixed apertures have inhomogeneous illumination. Therefore, angular current density measurements through a fixed aperture record averaged angular current density. This makes comparison of data difficult as averaged angular current density depends on aperture size. For the same reasons, voltage normalization cannot be performed for fixed aperture measurements except for aperture sizes that are infinitely small. Consistent determination of angular current density and voltage normalization, however, can be achieved if the beam diameter as well as total ion current are known. In cases where beam profile cannot be directly imaged with a field ion microscope, the beam profile could be extracted from measurements taken at multiple acceleration voltages and/or with multiple aperture sizes.

We demonstrate the combined use of large area depth-profiling dislocation imaging and quantitative composition and strain measurement for a strained Si/SiGe/Si sample based on nondestructive techniques of electron beam-induced current (EBIC) and X-ray diffraction reciprocal space mapping (XRD RSM). Depth and improved spatial resolution is achieved for dislocation imaging in EBIC by using different electron beam energies at a low temperature of ~7 K. Images recorded clearly show dislocations distributed in three regions of the sample: deep dislocation networks concentrated in the “strained” SiGe region, shallow misfit dislocations at the top Si/SiGe interface, and threading dislocations connecting the two regions. Dislocation densities at the top of the sample can be measured directly from the EBIC results. XRD RSM reveals separated peaks, allowing a quantitative measurement of composition and strain corresponding to different layers of different composition ratios. High-resolution scanning transmission electron microscopy cross-section analysis clearly shows the individual composition layers and the dislocation lines in the layers, which supports the EBIC and XRD RSM results.

The directional dark-field signal obtained with X-ray grating interferometry yields direction-dependent information about the X-ray scattering taking place inside the examined sample. It allows examination of its morphology without the requirement of resolving the micrometer size structures directly causing the scattering. The local morphology in turn gives rise to macroscopic mechanical properties of the investigated specimen. In this study, we investigate the relation between the biomechanical elasticity (Young’s modulus) and the measured directional dark-field parameters of a well-defined sample made of wood. In our proof-of-principle experiment, we found a correlation between Young’s modulus, the average dark-field signal, and the average dark-field anisotropy. Hence, we are able to show that directional dark-field imaging is a new method to predict mechanical sample properties. As grating interferometry provides absorption, phase-contrast, and dark-field data at the same time, this technique appears promising to combine imaging and mechanical testing in a single testing stage. Therefore, we believe that directional dark-field imaging will have a large impact in the materials science world.

An innovative approach, combining field-emission scanning electron microscopy (FESEM) with energy dispersive X-ray spectroscopy (EDX) analysis, is presented to investigate the degradation mechanisms affecting tannin-dyed wool. In fact, tannin-dyed textiles are more sensitive to degradation then those dyed with other dyestuffs, even in the same conservation conditions.

FESEM-EDX was first used to study a set of 48 wool specimens (artificially aged) dyed with several raw materials and mordants, and prepared according to historical dyeing recipes. EDX analysis was performed on the surface of wool threads and on their cross-sections. In addition, in order to validate the model formulated by the analysis of reference materials, several samples collected from historical and archaeological textiles were subjected to FESEM-EDX analysis.

FESEM-EDX investigations enabled us to reveal the correlation between elemental composition and morphological changes. In addition, aging processes were clarified by studying changes in the elemental composition of wool from the protective cuticle to the fiber core in cross-sections. Morphological and elemental analysis of wool specimens and of archaeological and historical textiles showed that the presence of tannins increases wool damage, primarily by causing a sulfur decrease and fiber oxidation.

This paper presents a method developed to quantify three-dimensional energy dispersive spectrometry (3D EDS) data with voxel size smaller than the volume from which X-rays are emitted. The influence of the neighboring voxels is corrected by applying recursively a complex quantification, improving thereby the accuracy of the quantification of critically small features. The enhanced quantification method is applied to simulated and measured data. A systematic improvement is obtained compared with classical quantification, proving the concept and the prospect of this method.

A test material for routine performance evaluation of energy-dispersive X-ray spectrometers (EDS) is presented. It consists of a synthetic, thick coating of C, Al, Mn, Cu, and Zr, in an elemental composition that provides interference-free characteristic X-ray lines of similar intensities at 10 kV scanning electron microscope voltage. The EDS energy resolution at the C-K, Mn-Lα, Cu-Lα, Al-K, Zr-Lα, and Mn-Kα lines, the calibration state of the energy scale, and the Mn-Lα/Mn-Kα intensity ratio as a measure for the low-energy detection efficiency are calculated by a dedicated software package from the 10 kV spectrum. Measurements at various input count rates and processor shaping times enable an estimation of the operation conditions for which the X-ray spectrum is not yet corrupted by pile-up events. Representative examples of EDS systems characterized with the test material and the related software are presented and discussed.

A procedure has been developed to follow degradation of energy-dispersive spectroscopy (EDS) X-ray lateral resolution in a variable pressure scanning electron microscope. This procedure is based on evaluation of the EDS profile shape change for different experimental conditions. Some parameters affecting the X-ray resolution in high-vacuum mode have been taken into account. Good agreement between the simulated and experimental EDS profiles shows the reliability of the proposed procedure. A significant improvement in measurement of the EDS profile interfacial distance (DINT) has been achieved.

A new in situ Scanning Electron Microscope-Focused Ion Beam-based method to study porous carbon electrodes involving Pt filling of pores from gaseous precursors has been demonstrated to show drastically improved image contrast between the carbon and porous phases when compared with the Si-resin vacuum-impregnation method. Whereas, the latter method offered up to 20% contrast, the new method offers remarkably higher contrast (42%), which enabled fast semi-automated demarcation of carbon boundaries and subsequent binarization of the images with very high fidelity. Tomographic reconstruction of the porous carbon electrode was then obtained from which several morphological parameters were quantified. The porosity was found to be 72±2%. The axial and radial tortuosites were 1.45±0.04 and 1.43±0.04, respectively. Pore size, which is defined to be the distance from the medial axis of the pore to the nearest solid boundary, was quantified. Average pore size determined from the pore size distribution was 90 nm and the corresponding 1 sigma ranges from 45 to 134 nm. Surface-to-volume ratio of the carbon phase was 46.5 µm−1. The ratio of total surface area to the total volume of electrode including pores (i.e., specific surface area) was 13 µm−1.

A versatile method to fabricate taper-free micro-/nanopillars of large aspect ratio was developed with focused ion beam (FIB) cutting. The key features of the fabrication are a FIB with an incident angle of 90° to the long axis of the pillar that enables milling of the pillar sideways avoiding tapering and the FIB current can be reduced step by step so as to reduce possible radiation damage of the milled surface by Ga ions. A procedure to accurately determine the cross-section of each pillar was developed.

An alternative focused ion beam preparation method is used for sampling historical photographs containing metallic nanoparticles in a polymer matrix. We use the preparation steps of classical ultra-microtomy with an alternative final sectioning with a focused ion beam. Transmission electron microscopy techniques show that the lamella has a uniform thickness, which is an important factor for analytical transmission electron microscopy. Furthermore, the method maintains the spatial distribution of nanoparticles in the soft matrix. The results are compared with traditional preparation techniques such as ultra-microtomy and classical focused ion beam milling.

Some image analysis techniques are developed for simplifying lattice fringe images of deposited pyrocarbon in carbon/carbon composites by chemical vapor infiltration. They are mainly the object counting method for detecting the optimum threshold, the self-adaptive morphological filtering, the node-separation technique for breaking the aggregate fringes, and some post processing algorithms for reconstructing the fringes. The simplified fringes are the foundation for defining and extracting quantitative nanostructure parameters of pyrocarbon. The frequency filter window of a Fourier transform is defined as the circular band that retains only those fringes with interlayer distance between 0.3 and 0.45 nm. Some judge criteria are set to define topological relation between fringes. For example, the aspect ratio and area of fringes are employed to detect aggregate fringes. Fringe coaxality and distance between endpoints are used to judge the disconnected fringes. The optimum values are determined by using the iterative correction techniques. The best cut-off value for the short fringes is chosen only when there is a reasonable match between the mean fringe length and the value measured by X-ray diffraction. The adopted techniques have been verified to be feasible and to have the potential to convert the complex lattice fringe image to a set of distinct fringe structures.

Transmission electron microscopes regularly produce data which has a dynamic range that exceeds the capabilities of the recording media used, particularly in diffraction patterns. Hardware solutions such as readable phosphor imaging plates have existed since the 1990s, but in recent years the advent of robust CCD digital cameras capable of capturing high intensities in a transmission electron microscope has made image acquisition fast and straightforward. However, all CCD cameras have a saturation limit, making imaging of low intensities difficult when an image is dominated by strong features. Here we present a simple and effective tool to overcome this limitation through acquisition of multiple images and software processing to produce high dynamic range electron images.

Fluctuation electron microscopy can reveal the nanoscale order in amorphous materials via the statistical variance in the scattering intensity as a function of position, scattering vector, and resolution. However, several sources of experimental artifacts can seriously affect the magnitude of the variance peaks. The use of a scanning transmission electron microscope for data collection affords a convenient means to check whether artifacts are present. As nanodiffraction patterns are collected in serial, any spatial or temporal dependence of the scattering intensity across the series can easily be detected. We present examples of the major types of artifact and methods to correct the data or to avoid the problem experimentally. We also re-cast the statistical formalism used to identify sources of noise in view of the present results. The present work provides a basis on which to perform fluctuation electron microscopy with a high level of reliability and confidence in the quantitative magnitude of the data.

Elimination of the electrostatic objective lens and alternative use of a Cc- and Cs-corrected quadrupole doublet may increase the useful working distance of the helium microscope, improve its resolution from 3 to 0.3 Å, and improve its optimum convergence angle from 0.4 to 4 mrad.