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The electron source brightness is an important parameter of an electron microscope. Reliable and easy brightness measurement routes are not easily found. A determination method for the illumination semi-angle distribution in transmission electron microscopy is even less well documented. Herein, we report a facile measurement route for both entities and demonstrate it on a state-of-the-art instrument. The reduced axial brightness of the FEI X-FEG with a monochromator was determined to be larger than 108 A/(m2 sr V).
Electron-beam (e-beam) irradiation damage is often regarded as a severe limitation to atomic-scale study of two-dimensional (2D) materials using electron microscopy techniques. However, energy transferred from the e-beam can also provide a way to modify 2D materials via defect engineering when the interaction of the beam with the sample is precisely controlled. In this article, we discuss the atomic geometry, formation mechanism, and properties of several types of structural defects, ranging from zero-dimensional point defects to extended domains, induced by an e-beam in a few representative 2D materials, including graphene, hexagonal boron nitride, transition-metal dichalcogenides, and phosphorene. We show that atomic as well as line defects and even novel nanostructures can be created and manipulated in 2D materials by an e-beam in a controllable manner. Phase transitions can also be induced. The e-beam in a (scanning) transmission electron microscope not only resolves the intrinsic atomic structure of materials with defects, but also provides new opportunities to modify the structure with subnanometer precision.
Group III nitrides are promising materials for light emitting diodes (LEDs). The occurrence of structural defects strongly affects the efficiency of these LEDs. We investigate the optical properties of basal plane stacking faults (BFSs), and the assignment of specific spectral features to distinct defect types by direct correlation of localized emission bands measured by cathodoluminescence in a scanning electron microscope with defects found in high resolution (scanning) transmission electron microscopy and electron beam induced current at identical sample spots. Thus, we are able to model the electronic structure of BSFs addressing I1, I2, and E type BSFs in GaN and AlGaN with low Al content. We find hints that BSFs in semipolar AlGaN layers cause local changes of the Al content, which strongly affects the usability of AlGaN as an electron blocking layer in nitride based LEDs.
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.
It is demonstrated that energy-filtered transmission electron microscope enables following of in situ changes of the Ca-L2,3 edge which can originate from variations in both local symmetry and bond lengths. Low accelerating voltages of 20 and 40 kV slow down radiation damage effects and enable study of the start and finish of phase transformations. We observed electron beam-induced phase transformation of single crystalline calcite (CaCO3) to polycrystalline calcium oxide (CaO) which occurs in different stages. The coordination of Ca in calcite is close to an octahedral one streched along the <111> direction. Changes during phase transformation to an octahedral coordination of Ca in CaO go along with a bond length increase by 5 pm, where oxygen is preserved as a binding partner. Electron loss near-edge structure of the Ca-L2,3 edge show four separated peaks, which all shift toward lower energies during phase transformation at the same time the energy level splitting increases. We suggest that these changes can be mainly addressed to the change of the bond length on the order of picometers. An important pre-condition for such studies is stability of the energy drift in the range of meV over at least 1 h, which is achieved with the sub-Ångström low-voltage transmission electron microscope I prototype microscope.
Specimen quality is vital to (scanning) transmission electron microscopy (TEM) investigations. In particular, thin specimens are required to obtain excellent high-resolution TEM images. Conventional focused ion beam (FIB) preparation methods cannot be employed to reliably create high quality specimens much thinner than 20 nm. We have developed a method for in situ target preparation of ultrathin TEM lamellae by FIB milling. With this method we are able to routinely obtain large area lamellae with coplanar faces, thinner than 10 nm. The resulting specimens are suitable for low kV TEM as well as scanning TEM. We have demonstrated atomic resolution by Cs-corrected high-resolution TEM at 20 kV on a FIB milled Si specimen only 4 nm thick; its amorphous layer measuring less than 1 nm in total.
A recent report on the “room temperature superplasticity” in the Zr64.13Cu15.75Ni10.12Al10 bulk metallic glass [Y.H. Liu et al., Science315, 1385 (2007)] was ascribed to the distinctive micrometer-sized structural heterogeneity. To verify the microstructure in this alloy, transmission electron microscopy (TEM) and anomalous small-angle x-ray scattering experiments were conducted. The results show that no micrometer-sized or nanometer-sized structural heterogeneities can be found. The micrometer-sized dark and bright regions that were previously reported as the reason for the plasticity are artifacts caused by TEM specimen preparation, rather than the intrinsic structure feature of this alloy. This finding is important for further studying the unique properties of this alloy.
A method is presented for recognition of nanograins in high-resolution transmission electron microscope (HRTEM) images of nanocrystalline materials. We suggest a numerical procedure, which is similar to the experimental dynamic hollow cone dark-field method in transmission electron microscopy and the annular dark-field method in scanning transmission electron microscopy. The numerical routine is based on moving a small mask along a circular path in the Fourier spectrum of a HRTEM image and performing at each angular step an inverse Fourier transform. The procedure extracts the amplitude from the Fourier reconstructions and generates a sum picture that is a real space map of the local amplitude. From this map, it is possible to determine both the size and shape of the nanograins that satisfy the selected Bragg conditions. The possibilities of the method are demonstrated by determining the grain size distribution in gadolinium with ultrafine nanocrystalline grains generated by spark plasma sintering.
Ethylene glycol modified precursors, such as tetrakis(2-hydroxyethyl)orthosilicate (EGMS) or bis(2-hydroxyethyl)titanate (EGMT), have distinct advantages in the synthesis of mesoporous materials by sol-gel processing compared to the commercially available tetraalkoxide precursors. The glycols released upon hydrolysis have proven to be compatible with lyotropic surfactant mesophases and in addition, these precursors allow for processing in purely aqueous conditions. Besides the standard characterization of the resulting titania and silica-based materials by XRD, electron microscopy, and nitrogen sorption, the potential of the titania-based materials for catalytic applications was tested using Au/TiO2 catalysts in low temperature CO oxidation reactions.