Crystallization of intergranular glass films can influence the performance of ceramic materials [1]. The crystallization of anorthite glass films has been studied in situ in the transmission electron microscope (TEM) [2]. The films are grown by pulsed-laser deposition (PLD) on sapphire (α-AI2O3) substrates. These substrates can be pre-thinned to electron transparency, so that contamination or microstructural damage of the TEM specimen due to the thinning process can be eliminated. This process also allows the microstructure of the glass films to be characterized before crystallization; the evolution of specific features of the film can then be tracked through repeated heat treatments. Prior to the crystallization of the anorthite glass films, observations confirmed that all the glass films deposited by PLD are indeed amorphous. Crystallization experiments were performed in a Philips CM30 TEM equipped with a Gatan single-tilt heating holder. Each specimen was heated in the microscope to a temperature of about 1200 °C at a heating rate of about 30 °C/min. and held at this temperature for 20 minutes.

It is well known that diffusion in ionic materials occurs primarily by the movement of charged species. Therefore, an applied electric field can provide a very large driving force for mass transport. In the present study, thin films of In2O3 and Fe2O3 have been deposited on (001) and (111) MgO using pulsed-laser deposition (PLD). These thin-film diffusion couples have then been reacted in an applied electric field at elevated temperatures. The electric field directly influences the diffusion of the cations in the constitutive layers. Through the use of both transmission (TEM) and scanning (SEM) electron microscopy, diffusion couples reacted either with and without an electric field have been analyzed to examine the effect that an induced ionic current can have on solid-state reaction processes.

The apparatus for reacting the diffusion couples in a field has been described elsewhere. The diffusion couples were characterized in cross-section by SEM and TEM techniques.

HRTEM images of α-Al2O3 oriented along [1100] often exhibit a modulation of the basal fringe intensity with a period that corresponds to twice the basal plane spacing. In the example shown in figure 1, note the strong basal fringe contrast in the A12O3 with a period of 4.33 Å. HRTEM image simulations for ideal imaging conditions fail to reproduce this doubling of the lattice fringe period. Instead, simulated images predict that the (0006) fringes (d0006=2.17 Å) should be of equal intensity (e.g., see Figure 3a). Incorrect beam and/or crystal tilt can strongly affect HRTEM image contrast. In particular, anomalous periodicities can arise under beam and crystal tilt conditions for which normally kinematically and dynamically forbidden diffracted beams contribute to the image. More recently, the importance of 3-fold astigmatism on HRTEM imaging has been recognized. As with beam tilt, this lens aberration produces asymmetrical phase shifts in the diffracted beams.

Layer silicates are important and abundant minerals. Polytypic details can be determined directly from atomic-resolution images recorded down [010] of layer silicates such as chlorite (Fig. 1), serpentine, and micas using a transmission electron microscope with a point resolution of ∼ 0.2 nm. For chlorite, this involves determination of whether octahedral slants in the brucite-like interlayers and octahedral sheet of the tetrahedral - octahedral-tetrahedral (TOT) layers are the same or opposed, the (3 angle, and how the octahedral cations in the brucite-like interlayer are positioned relative to the tetrahedral cations in the TOT layer (Fig. 1). Images must be recorded from the thinnest areas in order to distinguish slant of the brucite-like interlayer (composition dependent, but always < 0.7 nm sample thickness; 1). Polytype analysis is aided significantly by rotational filtering of images from thin areas to remove the amorphous contribution (2). All six of the common, semi-randomly stacked chlorite polytypes can be distinguished (1).

Since its invention inl982 scanning probe microscopy (SPM) has become an important analytical tool in every branch of physical science. The two most widely used types of SPM are atomic force Microscopy (AFM) and scanning tunneling microscopy (STM). Both AFM and STM allow measurement of the microtopography of a surface down to the atomic scale. Many spin-off applications such as lateral force and magnetic force allow measurement of a variety of the physical properties of a surface while imaging its microtopography. SPM can be done in both air and liquid and hence can be used to observe the interactions that take place at a solid-solution interface.

SPM has been used in mineralogy and geochemistry since 1989. Here as in other applications the great strength of SPM is in the characterization of the heterogeneous nature of mineral surfaces and the ability to observe many geochemical processes in real time.

Meteorites are remnants of the primordial material from which the solar system condensed. Most meteorites originated in the asteroid belt between Mars and Jupiter and fell to earth when their orbits were disturbed by collisions. Metal phases are present in all types of meteorites and are alloys of Fe and Ni containing S and P. The study of metal meteorites has yielded valuable information about the early thermal history of the solar system, since their heat treatment has been preserved in the microstructure and microchemistry of the meteorites and can be discerned by electron microscopy and microanalysis. A full understanding of the structure and chemistry of meteorites requires detailed knowledge of the Fe-Ni, Fe-Ni-S and Fe-Ni-P phase diagrams and determination of these diagrams has been carried out over more than three decades of electron-beam analysis by the authors.

The martian meteorite ALH84001 leapt into the spotlight in late 1996 when a NASA-led research team suggested that it contained evidence of biotic activity on ancient Mars. ALH84001 is unique among the martian meteorites- a cumulate rock made up predominantly of orthopyroxene, with interstitial maskelynite (feldspar turned into a diaplectic glass by shock), apatite, chromite and sulfides. Highly brecciated fracture zones cut through the rock, presumably a result of impacts, and within these zones is a variable amount of secondary carbonate. This carbonate, the most extensive secondary mineral found in any martian meteorite, formed during significant interaction between martian crust and volatiles, and represents a unique access point toward understanding the environment of ancient Mars. However, the conditions under which this carbonate formed are less clear. While claims for evidence of biotic activity are predicated on carbonate formation at low (<100°C) temperatures under water-rich conditions, other research suggests much less hospitable conditions, with little water present and formation temperatures approaching 700°C.

The technique of photo-electron emission microscopy (PEEM) is based on imaging of photo excited electrons from a surface. Typically ultra violet (UV) light above the work function of a metal will cause electrons to be emitted from a surface. Since photo excited electrons originate very near to the surface, they essentially reflect the electronic structure of the surface. These electrons may be accelerated and imaged, and the image will reflect the properties of the surface.

While the PEEM technique has been understood in a basic sense for many years, it has been limited by the lack of high intensity UV light sources. The most crucial part of the electron imaging system for PEEM, the objective lens, is essentially the same as for the sister technique of low energy electron microscopy (LEEM), and advances in electron optics capabilities have been exploited both for LEEM and for PEEM.

To obtain a full and detailed understanding of the spatiotemporal dynamics of surface processes such as epitaxial growth, strain relaxation, phase transformations and phase transitions, chemisorption and etching, in situ real-time observations have proven to be invaluable. The development of two experimental techniques, i.e. Low Energy Electron Microscopy (LEEM) typically operating at electron energies below 10 eV, and Ultra-High-Vacuum Transmission Electron Microscopy (UHV-TEM) at several 100 keV, has made such in situ studies routinely possible. In many cases, the videodata obtained from such experiments are amenable to detailed, quantitative analysis, yielding statistical, kinetic and thermodynamic information that cannot be obtained in any other way.

I will discuss recent experimental developments, including the design and construction of a new and improved LEEM instrument. Figure 1 shows a schematic diagram of this new machine. There are several features that distinguishes this design from most other LEEMs. One is the use of a 90 degree deflection magnetic prism array,

Due to the submicron size of crystallographic defects, characterization of dislocations has been done. mostly by electron microscopy techniques. Transmission electron microscopy has generated invaluable structural information at the atomic scale. However, the influence of these electrically active defects on carrier transport can only be learned from lower resolution (∼ 1 μm) techniques such as electron beam induced current (EBIC) and photocurrent measurements. Near-field scanning optical microscopy (NSOM) is a novel optical technique that circumvents the diffraction limit. In this talk, we will present the application of NSOM to perform near-field photocurrent (NPC) measurements on strain-relaxed GeSi films on Si substrates to study the electrical activity of individual threading dislocations. Photoexcited carriers are generated locally by NSOM light and are collected by the builtin p-n junctions in the sample resulting in an external photocurrent. As the tip moves across the sample, topographic and NPC images were acquired simultaneously.

There is increasing interest in the quantitative characterization of nanometer-scale semiconductor alloy layers, such as those of SiGe or AlGaAs. Electron holography, which has the ability to detect small changes in mean inner potential Vo, can in principle provide information about local changes in composition. However, the measurement of absolute values of Vo is not always straightforward and values for only a few materials are known with confidence. In this study, we measure Vo for Ge using electron holography, and we compare our experimental data with calculations. The holographic approach that we use to measure Vo is described in the paper of Gajdardziska-Josifovska et al. The Ge samples were nominally 90° cleaved wedges from a <100> wafer. Holograms were recorded on a Philips CM200 FEG equipped with a Gatan 794 CCD camera, and data were obtained for several crystal tilts (determined from diffraction patterns) to assess dynamical contributions to the phases.

It is challenging to access the microscopic distribution of strain in subsurface systems with a lateral resolution better than 1 nm and an accuracy of about 10-3 because such measurements require the detection of displacements by 1 pm at near atomic resolution. Nevertheless, such measurements are commonly desirable, in particular, for the investigations of thin heteroepitaxial films. A particular method developed in the past extracted geometrical information from unit cells in lattice images to perform this task in thin layers of cubic quantum well structures. Strain relaxation in thin TEM samples may falsify such measurements and needs to be controlled. It is the purpose of this paper to describe a quantitative method to measure strain with the required accuracy and resolution in the more complex hexagonal systems. A AxGa1-xN/GaN heterostructure grown on a sapphire substrate was investigated. Local strain comes from compositional variations which alter the size of the unit cells that are shown in Figure 1.

Introduction: The “real” semiconductor processing world consists of the universe of industrial and government semiconductor laboratories and manufacturing facilities plus a small number of university departments with heavy funding from industry—or a consortium of the above. We are bombarded with reports of how the drive toward faster, denser, lower power consuming and more reliable semiconductor products will accelerate with time. The smallest features of today's devices have already shrunk from view in visible light microscopes! Electron microscopy studies of semiconductor device materials, interconnects, insulators, and device packaging materials play a vital role in these extraordinarily “high tech” and financially important arenas.

Shifting semiconductor analytical paradigms: For the most part, the analytical paradigm has shifted: from visible light microscopy to SEM analysis, at low magnification and high accelerating voltage… to much more sophisticated SEM analysis, at high resolution and/or low accelerating voltages… to the many variations of TEM available today… and to new types of scanning probe microscopy.

Extensive long range transport of copper has been observed in polycrystalline aluminum-copper (Al-Cu) interconnects subjected to accelerated electromigration testing. Cu depletion is believed to be the rate limiting factor for electromigration damage accumulation. It is not clear if this is also the case for Al-Cu interconnects with bamboo/near-bamboo microstructures. In order to understand this phenomenon, Cu transport under electromigration conditions in bamboo microstructures has to be characterized quantitatively. This paper describes the procedure used to determine Cu distributions on a series of bamboo test structures subjected to accelerated electromigration (EM) testing. Copper composition profiles were determined for these structures through the use of electron probe microanalysis (EPMA) techniques and customized corrections for non-standard interaction volumes.

Aluminum (0.5 wt.% Cu) interconnect test line structures were fabricated with four metal layers and surrounding silicon dioxide dielectric. Following EM testing, the samples were deprocessed to expose the test lines at metal layer three, as shown in Figure 1.

Perovskite manganites, which have the the general formula R1-xAxMnO3 (R = La, Pr, or Nd and A = Ca, Sr, Ba, or Pb), have generated much recent interest because they exhibit “colossal magnetoresistance” (CMR), i.e. a small change in an applied magnetic field dramatically changes the electrical resistance of the material. Materials that exhibit this effect are being developed for various field-sensing applications but currently, the mechanism by which CMR occurs is not known. Conduction in these materials is explained by the “double exchange” mechanism, where the conductivity is attributed to electrons hopping back and forth between neighboring manganes ions. Such hopping is a maximum when the magnetic moments of the magnese ions are aligned parallel and a minimum when they are aligned antiparallel. In short, these materials show metallic conductivity when they are ferromagnetic and insulating behavior when they are antiferromagnetic. Moreover, they change from metallic to insulating behavior as a function of temperature.

Tin dioxide (SnO2) with rutile type structure exhibits unique electronic and optical properties. In applications of this material as gas sensors, a film-type of SnO2 provides high ratio of surface area to volume and lead to high sensitivity and fast responses. It has been found that substrate material, deposition conditions, and annealing procedure may directly control the microstructure of thin films, hence control gas-sensing properties. In this paper, we present transmission electron microscopy (TEM) studies of the microstructure and crystal defects of tin oxide thin films on sapphire substrate with subsequent annealing at high temperatures.

Tin oxide thin films were deposited on the surface of sapphire by e-beam evaporation of high purity SnO2 (99.999%) at 350°C followed by annealing in air at 600°C - 700°C. Microstructures of the films were characterized by X-ray diffraction (XRD) and TEM techniques.

GaSe, a member of the III-VI compound semiconductors, and its related compounds have recently gained an considerable attention because of their high non-linear optical coefficients in the infrared ranges, making them candidates for second harmonic generation (SHG) materials[l,2]. While the optical properties of those materials in bulk form are quite promising, poor thermal and mechanical properties preclude their easy applications. In thin film devices, the thermal and mechanical properties are dominated by those of the substrate, therefore, heteroepitaxially grown thin films of GaSe and related materials on substrates such as GaAs, Si and A12O3 should enable their application in device structures. Development of such new generation of materials, however, require fundamental knowledge about the surface and interface structure that play decisive roles in the thin film crystallinity and materials properties.

The growth of high quality GaAs layers on single crystal Ge substrates has attracted a great deal of interest in recent years. Currently under development at NREL is the GaAs/GalnP-on-Ge high efficiency multi-junction solar cell. Unlike other heteroepitaxial systems such as GaAs-on-Si, physical properties such as the lattice parameter and thermal expansion coefficient of the Ge and GaAs are much closer. Further, Ge has a bandgap of 0.7 eV that makes it a suitable bottom cell in a multi-junction stack. However, the growth of GaAs on Ge is not a straightforward process, and little is known about the Ge surface and the nucleation of GaAs on Ge in the MOCVD environment. In this study, TEM results show that a number microstructural defects are associated with the Ge/GaAs interface and the initial stages of growth.

III-V nitrides grown on (0001) sapphire substrates often contain a very high density of defects; this high density is usually attributed to the poor lattice and thermal match between the nitride and the sapphire [1]. There is thus a need to understand the defect structures in these materials. In the present study, a microstructural characterization of MBE-grown GaN films on (0001) sapphire using various TEM techniques was performed to evaluate defect structures in this material. This paper will outline some of the different types of defects found in these films and suggest some possible mechanisms by which they were formed.

Cobalt disilicide (CoSi2) is an attractive contact material for Si1-xGex devices due to its low resistivity, low Schottky barrier, and good thermal and chemical stability. Previous studies have shown that blanket Co films on Si0.80Ge0.20 react at annealing temperatures of 700 °C to form CoSi, CoSi2 and a Ge-rich Si1-xGex alloy; no Co-Ge phases were found. The Co preferentially reacts with the Si, which can lead to Ge segregation and island formation. To gain a better understanding of cobalt silicide formation, an electron microscopy investigation of Co/Si1-xGex/Si was performed.

Si1-xGex films (x ≤ 0.3) 64 nm to 260-nm thick were grown by molecular beam epitaxy at 550 °C on phosphorus-doped Si <001> substrates. Co films ranging in thickness from 5 nm to 25 nm were electron-beam evaporated (evaporator base pressure < 6.67 x 10-8 Pa) at room temperature on the Si1-xGex films.