The recently discovered compound BeP2N4 that crystallizes in the phenakite-type structure has potential application as a high strength optoelectronic material. Therefore, it is important to analyze experimentally the electronic structure, which was done in the present work by monochromated electron energy-loss spectroscopy. The detection of Be is challenging due to its low atomic number and easy removal under electron bombardment. We were able to determine the bonding behavior and coordination of the individual atomic species including Be. This is evident from a good agreement between experimental electron energy-loss near-edge structures of the Be-K-, P-L2,3-, and N-K-edges and density functional theory calculations.

TEAM I is the final product of the Transmission Electron Aberration-corrected Microscope (TEAM) Project, a collaborative project funded by the Department of Energy with the goal of designing and building a platform for a next generation aberration-corrected electron microscope capable of image resolution of up to 50 pm. The TEAM instrument incorporates a number of new technologies, including spherical- and chromatic-aberration correction, an all-piezo-electric sample stage and an active-pixel direct electron detector. This article describes the functionality of this advanced instrumentation, its response to changes in environment or operating conditions, and its stability during daily operation within the National Center for Electron Microscopy user facility.

Extended abstract of a paper presented at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, August 1–5, 2004.

Real space, high-resolution transmission electron microscopy observations of Xe confined in nanometer size faceted cavities in Al yield information on both the inert gas and the matrix in which it is confined. At room temperature, Xe in such cavities can be liquid or an fcc solid. In larger cavities, Xe within can undergo melting and recrystallization. The Al surface energy can be deduced from the largest Xe nanocrystal at 300 K by setting the corresponding calculated Laplace pressure equal to the equilibrium pressure for melting of Xe, obtained from empirical bulk compression data. These surface energy values are 1.05 J m-2 for {111} facets and 1.10 Jm-2 for {200} facets. Because of the weak interactions, these values correspond to the surface tensions for Al at 300 K.

At room temperature, fluid Xe confined in small faceted cavities in aluminum has up to three ordered layers of Xe atoms at the Al interface. Conceptually in a three-dimensionally confined system of sufficiently small size, complete three-dimensional ordering of the fluid may occur. Molecular dynamics simulations have revealed that such ordering would result in fluid Xe confined to a small tetragonal volume solidifying as a body-centered cubic phase on compression.

In situ transmission electron microscopy is an established experimental technique that permits direct observation of the dynamics and mechanisms of dislocation motion and deformation behavior. In this article, we detail the development of a novel specimen goniometer that allows real-time observations of the mechanical response of materials to indentation loads. The technology of the scanning tunneling microscope is adopted to allow nanometer-scale positioning of a sharp, conductive diamond tip onto the edge of an electron-transparent sample. This allows application of loads to nanometer-scale material volumes coupled with simultaneous imaging of the material’s response. The emphasis in this report is qualitative and technique oriented, with particular attention given to sample geometry and other technical requirements. Examples of the deformation of aluminum and titanium carbide as well as the fracture of silicon will be presented.

Thin films of gold can be grown on {001} Ge single crystal substrates in two equivalent {110} orientation variants, related to each other by a 90° rotation about the surface normal. The morphology of the films is that of a mazed bicrystal, a polycrystalline film with many randomly distributed columnar grains in only two orientations. All grain boundaries are of the type S99 and display pure tilt character. In this work, we report on observations of the structural relaxation of these grain boundaries, with special emphasis on their characteristic behavior at the intersection with free surfaces and their evolution during thermal annealing.

Thin films of gold (Au) were grown on single crystal germanium (Ge) or silicon (Si) substrates using physical vapor deposition (PVD). The resulting microstructure was that of a mazed bicrystal in which two equivalent grain orientations, related to each other by a 90° rotation, are arranged in a morphology of irregularly shaped, convoluted grains. Quantitative morphological analysis showed a strong dependence of grain shape on size, with larger grains being more convoluted and smaller grains more compact. The evolution of grain size, anisotropy and shape during heating in the temperature range from 300-340 °C was studied by in-situ transmission electron microscopy (TEM).

The evolution of liquid lead (Pb) inclusions at grain boundaries in aluminum (Al) was investigated by direct in situ TEM observation in the temperature range from 330°–643°C, In agreement with earlier reports on quenched alloys, the characteristic contact angle of the lens-shaped grain boundary inclusions was found to be near 120°. This angle remained approximately constant over the entire temperature range, ruling out the possibility of a wetting transition. Coarsening of grain boundary inclusions was observed to proceed mainly by Ostwald ripening, although coalescence could also be observed. Inclusions at grain boundaries, at triple junctions, and at the intersection of grain boundaries with the foil surfaces adopted characteristic shapes that were shown to be equilibrium forms. At the highest temperatures, the grain boundaries were observed to detach from the inclusions and the interaction of a migrating grain boundary with inclusions could be observed.

A “map” of all possible high-resolution images may be simulated for a crystalline specimen in a chosen orientation for any particular transmission electron microscope (HRTEM). These maps are useful during experimental high-resolution electron microscopy and make it possible to locate optimum imaging conditions even for foil thicknesses beyond the weak-phase object limit. Although defects such as grain boundaries are not generally periodic, image maps of perfect crystal can be used to optimize defect contrast during operation of the microscope by reference to the image of the perfect crystal neighboring the defect.