The Ninth Frontiers of Electron Microscopy in Materials Science Conference (FEMMS 2003) was held October 5–10, 2003 at the Claremont Resort and Spa in Berkeley, CA. Major sponsors for this meeting included Lawrence Livermore National Laboratory, Argonne National Laboratory, Lawrence Berkeley National Laboratory, Brookhaven National Laboratory, Frederick Seitz Materials Research Laboratory, Oak Ridge National Laboratory, National Science Foundation, and University of California at Davis. Sponsors also included LEO Electron Microscopy Ltd. (Carl Zeiss SMT), E. A. Fischione, Inc., Gatan, Inc., Thermo NORAN (Thermo Electron Corp.), FEI Company, Hitachi-HHTA, JEOL USA, Inc., Seiko Instruments, and CEOS GmbH.

Electron tomography is a well-established technique for three-dimensional structure determination of (almost) amorphous specimens in life sciences applications. With the recent advances in nanotechnology and the semiconductor industry, there is also an increasing need for high-resolution three-dimensional (3D) structural information in physical sciences. In this article, we evaluate the capabilities and limitations of transmission electron microscopy (TEM) and high-angle-annular-dark-field scanning transmission electron microscopy (HAADF-STEM) tomography for the 3D structural characterization of partially crystalline to highly crystalline materials. Our analysis of catalysts, a hydrogen storage material, and different semiconductor devices shows that features with a diameter as small as 1–2 nm can be resolved in three dimensions by electron tomography. For partially crystalline materials with small single crystalline domains, bright-field TEM tomography provides reliable 3D structural information. HAADF-STEM tomography is more versatile and can also be used for high-resolution 3D imaging of highly crystalline materials such as semiconductor devices.

Indirect high resolution electron microscopy using one of several possible data-set geometries offers advantages over conventional high-resolution imaging in enabling the recovery of the complex wavefunction at the specimen exit plane and simultaneously eliminating the aberrations present in the objective lens. This article discusses results obtained using this method from structures formed by inorganic materials confined within the bores of carbon nanotubes. Such materials are shown to be atomically regulated due to their confinement, leading to integral layer architectures that we have termed “Feynman crystals.” These one-dimensional (1D) crystals also show a wide range of structural deviations from the bulk, including unexpected lattice distortions, and in some cases entirely new forms have been observed.

Nanophase aluminum powder was characterized in a field-emission-gun transmission electron microscope (TEM). Different techniques were used to investigate the structure of the particles, including conventional bright-field and dark-field imaging, scanning transmission electron microscopy (STEM), high-resolution lattice imaging, diffraction studies, energy dispersive X-ray spectroscopy (EDS) analysis and mapping, and electron energy loss spectroscopy (EELS) analysis and mapping. It has been established that the particle cores consist of aluminum single crystals that sometimes contain crystal lattice defects. The core is covered by a passivating layer of aluminum oxide a few nanometers thick. The alumina is mostly amorphous, but evidences of partial crystallinity of the oxide were also found. The thickness of this layer was measured using different techniques, and the results are in good agreement with each other. The particles are agglomerated in two distinct ways. Some particles were apparently bonded together during processing before oxidation. These mostly form dumbbells covered by a joint oxide layer. Also, oxidized particles are loosely assembled into relatively large clusters.

The novel crystallization properties of nano-materials represent a great challenge to researchers across all disciplines of materials science. Simple binary solids can be found to adopt unprecedented structures, when confined into nanometer-sized cavities, such as the inner cylindrical bore of single-walled carbon nanotubes (SWNT). Lanthanum iodide was encapsulated within SWNTs and the resulting encapsulation composite was analyzed using energy-dispersive X-ray microanalysis (EDX) and high-resolution transmission electron microscopy (HRTEM) imaging techniques, to reveal a one-dimensional crystal fragment, with the stoichiometry of LaI2, crystallizing in the structure of LaI3 with one third of the iodine positions unoccupied. A complete characterization of the encapsulation composite was achieved using an enhanced image restoration technique, which restores the object wave from a focal series of HRTEM images, providing information about the precise structural data of both filling material and host SWNT, and thereby enabling the identification of the SWNT chirality.

Practical analyses of the structures of ultrathin multilayers in tunneling magneto resistance (TMR) and Magnetic Random Access Memory (MRAM) devices have been a challenging task because layers are very thin, just 1–2 nm thick. Particularly, the thinness (∼1 nm) and chemical properties of the AlOx barrier layer are critical to its magnetic tunneling property. We focused on evaluating the current TEM analytical methods by measuring the thickness and composition of an AlOx layer using several TEM instruments, that is, a round robin test, and cross-checked the thickness results with an X-ray reflectometry (XRR) method. The thickness measured by using HRTEM, HAADF-STEM, and zero-loss images was 1.1 nm, which agreed with the results from the XRR method. On the other hand, TEM-EELS measurements showed 1.8 nm for an oxygen 2D-EELS image and 3.0 nm for an oxygen spatially resolved EELS image, whereas the STEM-EDS line profile showed 2.5 nm in thickness. However, after improving the TEM-EELS measurements by acquiring time-resolved images, the measured thickness of the AlOx layer was improved from 1.8 nm to 1.4 nm for the oxygen 2D-EELS image and from 3.0 nm to 2.0 nm for the spatially resolved EELS image, respectively. Also the observed thickness from the EDS line profile was improved to 1.4 nm after more careful optimization of the experimental parameters. We found that EELS and EDS of one-dimensional line scans or two-dimensional elemental mapping gave a larger AlOx thickness even though much care was taken. The reasons for larger measured values can be found from several factors such as sample drift, beam damage, probe size, beam delocalization, and multiple scattering for the EDS images, and chromatic aberration, diffraction limit due to the aperture, delocalization, alignment between layered direction in samples, and energy dispersion direction in the EELS instrument for EELS images. In the case of STEM-EDS mapping with focused nanoprobes, it is always necessary to reduce beam damage and sample drift while trying to maintain the signal-to-noise (S/N) ratio as high as possible. Also we confirmed that the time-resolved TEM-EELS acquisition technique improves S/N ratios of elemental maps without blurring the images.

The damage layers generated in III–V compounds exposed to energetic gallium ions in a focused ion beam (FIB) instrument have been characterized by transmission electron microscopy (TEM). The damage on the side walls of the milled trenches is in the form of amorphous layers associated with direct amorphization from the gallium beam, rather than from redeposition of milled material. However, the damage on the bottom of the milled trenches is more complex. For InP and InAs the damage layers include the presence of crystalline phases resulting from recrystallization associated heating from the incident beam and gallium implantation. In contrast, such crystalline phases are not present in GaAs. The thicknesses of the damage layers are greater than those calculated from theoretical models of ion implantation. These differences arise because the dynamic nature of FIB milling means that the energetic ion beams pass through already damaged layers. In InP recoil phosphorus atoms also cause significant damage.

Analytical transmission electron microscopy (TEM) and scanning electron microscopy (SEM) have been applied for the characterization of evolution, lateral arrangements, orientations, and the microscopic nature of nanostructures formed during the early stages of ultrahigh vacuum electron beam evaporation of Cu onto surfaces of VSe2 layered crystals. Linear nanostructure of relatively large lateral dimension (100–500 nm) and networks of smaller nanostructures (lateral dimension: 15–30 nm; mesh sizes: 500–2000 nm) are subsequently formed on the substrate surfaces. Both types of nanostructures are not Cu nanowires but are composed of two strands of crystalline substrate material elevating above the substrate surface. For the large nanostructures a symmetric roof structure with an inclination angle of ∼30° with respect to the substrate surface could be deduced from detailed diffraction contrast experiments. In addition to the nanostructure networks a thin layer of a Cu-VSe2 intercalation phase of 3R polytype is observed at the substrate surface. A dense network of interface dislocations indicates that the phase formation is accompanied by in-plane strain. We present a model that explains the formation of large and small nanostructures as consequences of compressive layer strains that are relaxed by the formation of rooflike nanostructures, finally evolving into the observed networks with increasing deposition time. The dominating contributions to the compressive layer strains are considered to be an electronic charge transfer from the Cu adsorbate to the substrate and the formation of a Cu-VSe2 intercalation compound in a thin surface layer.

diFiore's Atlas of Histology with Functional Correlations. Victor P. Eroschenko. Lippincott Williams and Wilkins, Philadelphia, PA; 10th edition, 2005, 448 pages (Softbound and Software CD (interactive), $57.95), ISBN 0-7817-5021-0

Histology (or microscopic anatomy) is an important discipline of the biological sciences that is concerned with the structure of tissues of organisms. Light microscopy and electron microscopy in conjunction with various histochemical and immunocytochemical staining techniques are typically used today by histologists to visualize, describe, and identify tissues. Histology is a fundamental discipline in the curriculum for medical, dental, and veterinary students as well as for allied health students and scholars interested in the field of biomedical research. All these students need to have a thorough knowledge of the structure and function of cells, tissues, and organs. Recently, I came across a histology book (diFiore's Atlas of Histology) that I believe is worth the investment. This book provides a selection of high-quality, full-color illustrations of various tissues of the human body and is supplemented with sections of structural/functional correlations. This 10th edition is unique in that it includes a CD that contains an interactive electronic version of the histology atlas.

The following shows the correction to Equation (3) that appeared on page 356 of Microscopy and Microanalysis, 11:4, August 2005, in the article by Admon et al. The lines, highlighted with gray screen, were inadvertently left out.

Date Change: Microscopy & Microanalysis 2006 will take place July 30–August 3, 2006 in Chicago, IL. Please disregard previously listed dates.

Following is a list of microscopy-related meetings and courses. The editors would greatly appreciate input to this list via the electronic submission form found in the MSA World-Wide Web page at http://www.msa.microscopy.com. We will gladly add hypertext links to the notice on the web and insert a listing of the meeting in the next issue of the Journal. Send comments and questions to JoAn Hudson, joanh@clemson.edu or Nestor Zaluzec, zaluzec@aaem.amc.anl.gov.