This issue marks the beginning of the 15th year of publication for Microscopy and Microanalysis (MAM), and it is my pleasure and honor to start my tenure as Editor-in-Chief of the journal with Volume 15, 2009. The idea for this scientific journal originated during Charles Lyman's term as president of the Microscopy Society of America in 1991, and in 1992 a peer-reviewed demonstration issue was published as vol. 22, no. 1 of the MSA Bulletin. After evaluating several publishing formats, a new peer-reviewed journal was launched in 1995 as the Journal of the Microscopy Society of America. When Springer-Verlag became the publisher in 1997, the title of the journal was changed to Microscopy and Microanalysis. In 2002, publication moved to Cambridge University Press (CUP) and in 2006 the CUP Managing Editor, Ed Barnas, and the MAM Editor-in-Chief, Charles Lyman, moved manuscript submission for the journal to the electronic submission site “Manuscript Central” operated by ScholarOne. At the end of 2008, Charles Lyman retired from the journal having served as MAM Editor for 12 years and Editor-in-Chief for 9 years.

Ultrastructure of the zona pellucida (ZP) of canine and feline oocytes has not been fully investigated. The objective of the study was to evaluate the potential use of the low vacuum scanning electron microscope (LVSEM) with oocytes. This required development of a method to prepare canine and feline cumulus-oocyte complexes (COCs) for LVSEM to provide ultrastructural information on the ZP. COCs were collected from ovaries, and cumulus cells were either partially or completely removed to reveal the ZP. COCs and zona-intact oocytes were fixed at 4°C for 1 h in 2.5% glutaraldehyde in 0.1 M sodium cacodylate buffer, pH 7.4 and subsequently viewed wet or further processed by critical point drying, and viewed uncoated or sputter coated with gold. Although the spongy surface of the ZP was visible at low vacuum in uncoated oocytes, coated oocytes had more details at high vacuum. The ZP surface of canine and feline oocytes contained numerous various-sized, spherical or elliptical pores that narrowed centripetally splitting into several smaller, deep pores. The round to oblong cumulus cells tightly surrounded the ZP. Each corona radiata cumulus cell tapered into a thin projection that entered the ZP. Our detailed techniques will enable future studies connecting ultrastructural and molecular aspects of oocyte maturation and development in mammals.

We present a fast and simple method to prepare specimens for transmission electron microscopy studies of oxide thin films deposited on silicon substrates. The method consists of scratching the film surface using a pointed diamond tip, in a special manner. Small and thin fragments are then detached from the film and its substrate. Depending on the scratching direction, the fragments can be used for plan-view or cross-section imaging. High-resolution images can be also obtained from thin edges of the film fragments. The method is demonstrated in the case of HfO2 sol-gel films deposited on [100] Si wafer substrates.

This series of articles describes a method that performs (semi)quantitative phase analysis for nanocrystalline transmission electron microscope samples from selected area electron diffraction (SAED) patterns. Volume fractions of phases and their textures are obtained separately in the method. First, the two-dimensional SAED pattern is converted into an X-ray diffraction–like one-dimensional distribution. Volume fractions of the nanocrystalline components are determined by fitting the spectral components, calculated for the previously identified phases with a priori known structures. Blackman correction is also applied to take into account dynamic effects for medium grain sizes. Peak shapes and experimental parameters (camera length, etc.) are refined during the fitting iterations. Parameter space is explored with the help of the Downhill-SIMPLEX algorithm. Part I presented the principles, while Part II now elaborates current implementation, and Part III will demonstrate its usage by examples. The method is implemented in a computer program that runs under the Windows operating system on IBM PC compatible machines.

This article discusses the results of transmission electron microscopy (TEM)-based characterization of strontium-doped lead zirconate titanate (PSZT) thin films. The thin films were deposited by radio frequency magnetron sputtering at 300°C on gold-coated silicon substrates, which used a 15 nm titanium adhesion layer between the 150 nm thick gold film and (100) silicon. The TEM analysis was carried out using a combination of high-resolution imaging, energy filtered imaging, energy dispersive X-ray (EDX) analysis, and hollow cone illumination. At the interface between the PSZT films and gold, an amorphous silicon-rich layer (about 4 nm thick) was observed, with the film composition remaining uniform otherwise. The films were found to be polycrystalline with a columnar structure perpendicular to the substrate. Interdiffusion between the bottom metal layers and silicon was observed and was confirmed using secondary ion mass spectrometry. This occurs due to the temperature of deposition (300°C) being close to the eutectic point of gold and silicon (363°C). The diffused regions in silicon were composed primarily of gold (analyzed by EDX) and were bounded by (111) silicon planes, highlighted by the triangular diffused regions observed in the two-dimensional TEM image.

The valence states of Mg-Al alloys are compared to those of reference materials (pure Mg and Al metals, and intermetallics). Two methods based on X-ray emission spectroscopy are proposed to determine the phases and their proportion: first, by analyzing the Al valence spectra of the Mg-rich alloys and the Mg valence spectra of the Al-rich alloys; second, by fitting with a linear combination of the reference spectra the Al spectra of the Al-rich alloys and the Mg spectra of the Mg-rich alloys. This enables us to determine that Al and Al3Mg2 are present in the 0–43.9 wt% Al composition range and Mg and Al12Mg17 are present in the 62.5–100 wt% Al composition range. In the 43.9–62.5% Al range, the alloy is single phase and an underestimation of the Al content of the alloy can be estimated from the comparison of the bandwidth of the alloy spectrum to the bandwidths of the reference spectra.

ZrO2:Yb3+ nanocrystalline phosphors with high concentrations of ytterbium ions were prepared using the sol-gel method. X-ray diffraction, high-angle annular-dark-field scanning transmission electron microscopy (HAADF-STEM), energy dispersive X-ray spectroscopy, and high-resolution transmission electron microscopy (HRTEM) were used to characterize the nanocrystalline phosphors annealed at 1000°C. Unit-cell distortion and changes in the crystalline structure of the monoclinic zirconia to tetragonal zirconia, and subsequently cubic zirconia, were observed with increased Yb concentration. Yb ions were randomly distributed into the lattice of the crystalline structure. No segregation of Yb2O3 phase was observed. The substitution of Zr atoms by Yb atoms on different crystalline phases was confirmed by the experimental results and theoretical simulations of HRTEM and HAADF-STEM.

We examine chemical mapping of reaction phases in a Cu-Al multilayer system using low-loss electron energy loss spectroscopy spectrum imaging and image spectroscopy techniques. The sensitivity of the plasmon peak position and shape to various crystal structures and phases is exploited using postprocessing of spectra into second derivative plasmon maps and line scans. Analytical transmission electron microscopy is complemented by studies of the orientation relationship of the multilayer system using high-resolution electron microscopy of interfaces and selected area diffraction. The techniques have been applied to the Cu-Al multilayer sample and sharply bound epitaxial phases are found, before and after heat treatment.

The microstructure of a 55 μm diameter, cold-worked Ni-Ti microwire is investigated by different transmission electron microscopy techniques. The surface consists of a few hundred nanometer thick oxide layer composed of TiO and TiO2 with a small fraction of inhomogeneously distributed Ni. The interior of the wire has a core-shell structure with primarily B2 grains in the 1 μm thick shell, and heavily twinned B19′ martensite in the core. This core-shell structure can be explained by a concentration gradient of the alloying elements resulting in a structure separation due to the strong temperature dependence of the martensitic start temperature. Moreover, in between the B2 part of the metallic core-shell and the oxide layer, a Ni3Ti interfacial layer is detected.

A method is described for quantitatively analyzing the level of interconnectivity of solid-oxide fuel cell electrode phases. The method was applied to the three-dimensional microstructure of a Ni–Y2O3-stabilized ZrO2 (Ni-YSZ) anode active layer measured by focused ion beam scanning electron microscopy. Each individual contiguous network of Ni, YSZ, and porosity was identified and labeled according to whether it was contiguous with the rest of the electrode. It was determined that the YSZ phase was 100% connected, whereas at least 86% of the Ni and 96% of the pores were connected. Triple-phase boundary (TPB) segments were identified and evaluated with respect to the contiguity of each of the three phases at their locations. It was found that 11.6% of the TPB length was on one or more isolated phases and hence was not electrochemically active.