A number of recent studies of grain boundaries and heterophase interfaces have demonstrated the power of combining Z-contrast STEM imaging, EELS and first-principles theoretical modeling to give an essentially complete atomic scale description of structure, bonding and energetics. Impurity sites and valence can be determined experimentally and configurations determined through calculations.

Here we present an investigation of the Si/SiO2 interface. The Z-contrast image in Fig. la, taken with the VG Microscopes HB603U STEM, shows that the atomic structure of Si is maintained up to the last layers visible. The decrease in intensity near the interface could originate from interfacial roughness of around one unit cell (∼0.5 nm), or may represent dechanneling in the slightly buckled columns induced by the oxide. Fig. lb, taken from a sample with ∼1 nm interface roughness, shows a band of bright contrast near the interface. This is not due to impurities or thickness variation since it disappears on increasing the detector angle from 25 mrad to 45 mrad (Fig. lc), and is therefore due to induced strain.

SIMS has inherent difficulties with quantification because of the so called “matrix effect”. Many factors contribute to the matrix effect, e.g. differing concentration of oxygen, sputtering rate differences in the hetero-layers, etc. In the case of MOS(metal-oxide-semiconductor) structures, the oxide layer gives rise to a large matrix effect. It is thus very difficult to use SIMS to evaluate the relationship between the electrical properties of the LSI devices and the impurity profiles present in such systems.

So we have been studying laser post-ionization SNMS, which consists of TOF-SIMS apparatus and excimer laser, in order to quantify the impurity profiles around SiO2/Si interface. Depth profiles of implanted Cu with 1×1015 atoms/cm2 in SiO2(100 nm)/Si system taken by Monte-Carlo simulation ,SIMS and laser post-ionization SNMS are shown in Fig.l. In this implantation condition the Cu+:Cu2+:Cu3+ percentage ratios of the charge distributions were 44:42:14. Fig. 1(a) shows the theoretical depth profiles expetted from this implantation condition by Monte-Cairo simulation.

Growth of germanium or silicon-germanium on silicon 100 surfaces produces pyramid shaped islands after several monolayers of coverage. With further deposition, these islands will continue to grow until they reach a critical volume where a transition to a dome shape occurs. The critical surface coverage for island formation and the critical volume for the pyramid to dome transition depend upon the silicon to germanium ratio or degree of mismatch between the deposited material and the silicon substrate. Strain plays a dominant role in the shape transitions. Annealing studies have shown that the pyramid to dome transition.is reversible and is likely due to strain reduction related to interdiffusion. Annealing results in island growth, a decrease in the number of islands, and interdiffusion of the silicon and germanium. The interdiffusion relieves the strain and shifts the critical volume to a value exceeding the current volume of the dome shaped island thereby driving the transition back to pyramidal shape.

Changes in electronic structure and bonding at metal-oxide interfaces can have a pronounced influence on the macroscopic properties of the interface. This is particularly true for supported-metal catalysts, which feature nanometer-sized transition metal particles dispersed on an inert support such as A12O3 or SiO2. Variations in the d-band filling of the transition metal due to chemical bonding with the support could potentially alter the chemical activity of metal atoms near the interface, thereby affecting catalyst performance. This work investigates possible interface contributions to the performance of a model Ni- SiO2 catalyst system by directly assessing the nature of bonding at the metal-oxide interface. Electron energy-loss spectrometry (EELS) in the TEM is used to examine and quantify changes in the d-band occupancy of interfacial Ni atoms relative to the bulk, and to further relate these changes to interface chemistry.

The Ni d-band occupancy is evaluated using the integrated area under the Ni L2,3 edge in the energyloss spectrum, according to routines establishe-i previously.

GaN is a direct, wide band -gap semiconductor (Eg =3.4 eV) which has a potential application in electronic and optical devices including UV-emitting lasers and bright p-n junction GaN light emitting diodes. In order to attain optimum device performance, it is necessary to develop lowresistance, thermally stable and uniform ohmic contacts.

In this study, the TiN/GaN contact synthesis and examination of contact performance were conducted at North Carolina State University. Si-doped n-GaN films were grown on 6H-SiC substrates via MOVPE with an A1N buffer layer. The TiN films were deposited in an ion-beam assisted, UHV electron-beam evaporation system. TiN growth was performed at a substrate temperature of 350 °C and a nitrogen pressure of about 2×10-4 torr. The deposition rate was 1- 1.5 nm/min. The TiN contacts deposited on (0001) n-GaN were ohmic with high resistivity in the as-deposited condition, but the resistivity decreased sharply in response to annealing. The TiN/GaN interface was examined by transmission electron microscopy to provide correlations between changes in microstructure and electrical behavior.

In this proceedings, we present a review of our experimental results of our investigations of the mechanisms of the initial stages of copper oxidation. We examined the initial stages of Cu(001) oxidation and reduction by in situ ultra-high vacuum (UHV) transmission, electron microscopy (TEM). We observed surface reconstruction and nucleation and growth of copper oxide islands. We have examined the oxidation processes from oxygen partial pressures of 10-5 torr to atmospheric pressures and temperatures from 25°C to 600°C, in order to gain fundamental insights into this important gas-metal reaction.

Fundamental knowledge of gas-metal reactions, in particular oxidation, is important for a wide variety of materials science fields, such as dry corrosion, catalysis, as well as some thin film growth, such as ferroelectrics. However, there is a wide gap between information provided by surface science methods and that provided by bulk oxidation studies. The former have mostly examined the adsorption of up to ˜1ML of oxygen on the metal surface.

Transmission electron microscopy plays a key role in the investigation of precipitates and inclusions because it provides direct information at high spatial resolution, on their shape, orientation relationship, interface structure and composition.

This work has utilized high resolution and in-situ electron microscopy to study the equilibrium shapes and thermal behavior of Pb precipitates in Al. It was found that PB precipitates within Al grains form in parallel-cube orientation relationship, are cuboctahedral in shape, adopt a sequence of magic sizes, and display an increase in aspect ratio with decreasing size. These observations have been explained in terms of interfacial energy and residual strain energy.

When the same Pb precipitates form on grain boundaries, their shapes are significantly different. This is apparent from figure 1 which shows a 90° <110> tilt grain boundary in Al with a small cuboctahedral Pb precipitate in the upper grain and a large complex-shaped Pb particle on the grain boundary.

Development of high-density longitudinal magnetic recording media (used for computer hard disks) with good noise performance and high thermal stability requires optimization of both alloy composition and processing methods. In CoCr(PtTa) thin films, intergranular Cr segregation is responsible for decoupling the magnetic exchange between the small ferromagnetic grains. The corresponding Cr depletion within the grains affects the “bulk” magnetic anisotropy. However, the nanoscale structural and chemical details that are needed for modeling and for guiding material development are not well understood. Energy-filtered transmission electron microscopy (EFTEM) has been used to characterize a series of CoCrTa/Cr, CoCrPt/Cr, and CoCrPtTa/Cr media sputtered under various processing conditions, in order to understand their structure-property-processing relationships.

Processing typical for hard-disk media was used: 30 or 60-nm films of a Cr underlayer followed by a Co alloy were d.c. magnetron sputtered onto a NiP-plated Al substrate pre-heated to 250°C.

The discovery of amorphous, or glassy, metallic alloys in 1959 posed an intellectual challenge. How can one describe the structure of glasses when there is no long-range periodicity? What can the structure tell us about why certain metal alloys form glasses more easily than others? First, some universal characteristics, if any exist, of the structure metallic glasses needed to be found. A convincing model was proposed for the structure of metallic glasses based on Bernal’s dense random packing (DRP) structure. Central to this proposal is the idea that the structure of metallic glasses is that of the random filling of space by non-interacting identical spheres. In this model, strongly directional interatomic bonds do not play an important role in determining the structure of metallic glasses. This model is hpwever in conflict with one proposed by Chen, which correlates increased glass formability with increased chemical interaction between dissimilar atoms.

Carbon nanotubes and carbon onions are two fascinating forms of crystalline nanosize carbons that have received considerable attention in recent years (1,2). The remarkable physical properties of nanotubes make them valuable material for applications ranging from electronic devices to nanoprobes. The dimensions and topology of these structures make them fascinating objects for study. Multiwalled nanotubes and onions are made of concentric graphite layers, with different geometry. Singlewalled nanotubes on the other hand are made of singular graphene cylinders, often self-assembled into larger rope-like structures. Nanotubes can be produced in gram quantities using electric arc or laser ablation. Carbon onions, however, are structures that assemble from carbonaceous soot under intense electron irradiation in an electron microscope. Hence the onions are metastable structures that become unstable and disintegrate in the absence of irradiation.

The multiwalled carbon nanotubes and carbon onions have been shown to encapsulate foreign materials (metals, oxides, carbides), either during growth or by capillarity filling (in the case of nanotubes) (1), or during irradiation of metal containing soot (onions) (3).

Supported Pt-metal catalysts are of immense commercial importance for hydrogenation reactions. The fine chemicals industry relies on special catalysts that selectively hydrogenate specific bonds or chemical functions on molecules. The activity, selectivity, lifetime, etc. of a supported hydrogenation catalyst is wellknown to depend strongly on the chosen support, but systematic studies of the role of the support and of support-metal interactions are lacking in the literature. The purpose of this work is to examine in detail the function of single-wall carbon nanotubes (SWNT) as support for a Pt catalyst, in the context of a selective hydrogenation reaction. The test reaction consists of the hydrogenation of the carbonyl group on 3-methyl-2- butenal, a reaction extensively studied on well-characterized Pt surfaces and also unsupported polycrystalline Pt. This reaction, which follows a parallel/consecutive reaction network (Fig. 1), represents a class of selective hydrogenation reactions of α,β-unsaturated aldehydes that are important in the fine chemicals industry for flavorings, fragrances, and some pharmaceuticals.

Single wall carbon nanotubes (SWNT) were doped with iodine, resulting in charge transfer between the iodine and carbon [1]. It was found that the iodine intercalation is air stable and also reversible by simple heat treatment. This behavior is in contrast to graphite and fullerenes which do not form charge transfer compounds with iodine. Although the iodine-induced charge transfer was not found in any other carbon polymorph solid, it has been found in some low dimensional organic polymers such as polyaniline,[2] forming charged linear-chain polyiodides (I3)- and (I5)-. This suggests that the geometric configuration of the carbon may play a very important role in iodine intercalation. In this study, we use Z-contrast imaging[3] in a VG Microscopes HB603U STEM to directly observe the configuration of iodine within the nanotube bundles. First-principles density-functional calculations are then used to explain the preference for the observed iodine configuration within the nanotubes.

The quantification of grain boundary segregation levels, as measured with X-ray energy dispersive spectroscopy (XEDS) in a scanning transmission electron microscope (STEM), is dependent on the size and shape of the interaction volume. The segregation level T (in atoms/nm2) is related to the intensities of the characteristic peaks in the X-ray spectrum, Is and Im, by

where ρ is the density of the matrix in atoms/nm3, Am and As are the atomic masses of the matrix and segregant respectively and ksm is the usual k-factor. The geometric factor, V/A, is the ratio of the volume of interaction to the area of the grain boundary inside in the interaction volume. Different models have been used to describe the interaction volume and these are illustrated in Fig. 1 and the appropriate expression for V/A is given in each case. In the simplest case, beam broadening is neglected and the interaction volume can be described as a cylinder with diameter equal to the probe size, d.

A lot of efforts have been devoted to understanding an interfacial structure. But, there are some difficulties about it as follows: An interfacial structure depends on a surface structure of a substrate and its temperature. Also, an interfacial structure is not homogeneous in general because of a lattice mismatch between a substrate and an overlayer thin film.

Ultrahigh vacuum transmission electron microscope (UHV-TEM) is very powerful to observe clean surface and the fabrication during deposition on the surface. Since structural information can be obtained from 10 nm-sized area to a few μm area using TEM, UHVTEM is very appropriate to investigate interfacial structure in detail.

In this study, structure of Ag/Si(111)--R30-Ag interface was observed by UHVTEM. Especially, it is interesting whether the superstructure is conserved at this interface or not. The Si(l11)- as the substrate surface was obtained by Ag 1ML deposition on Si(l11) 7×7 surface at 673 K.

Multilayer film (MLF) structures which exhibit giant-magnetoresistance (GMR) properties have applications in the areas of magnetic recording and computer memory. The magnetic properties of MLF structures are dependent upon structural and compositional variations at the atomic level. Thus, structural characterization with high spatial resolution, especially at layer interfaces, is important in order to optimize device performance with respect to processing and operating conditions. Atom probe field ion microscopy (APFIM) is one technique that has the capability to characterize the local structure and composition of MLF devices with sufficiently high resolution. However, a major difficulty has been successful specimen preparation from MLF materials, which requires fabrication of a sharply pointed needle (radius <50 nm) containing the layers of interest in the apex region. Research on specialized field ion specimen preparation techniques which use focused ion beam milling has recently enabled nanoscale MLF structures to be investigated. In the present paper, the application of atom probe microanalysis to two different MLF structures is presented.

One-, two- and three-layer polytypes are common in muscovite (sheet silicate). Based on high-resolution transmission electron microscopy (HRTEM) and analytical electron microscopy (AEM) examinations, we report in the discovery of complex 5-layer and 7- layer polytypes in natural muscovite for the first time (Fig. 1) and the implications of polytype transitions.

Three main structures are found in muscovite crystals in a sample from Oreana, Nevada, which are 1M, 2M1, and a disordered structure often containing short-range ordered stacking sequences. On the scale of a few micrometers, muscovite occurs as ordered crystals, disordered crystals, and crystals with regions of ordered and disordered layer stacking.

Short-range ordered 5- or 7-layer repeats are found in some disordered structures where single 4-, 6-, 9- or 10-layer intergrowths occur occasionally with 2- and 3-layer repeats. Such complex polytypes have not been observed before in either natural or synthetic muscovite, although 5- and 7-layer structures are commonly present in trioctahedral micas (i.e., biotite) (Baronnet, 1992).

SrTiO3-based semiconducting ceramics are widely used to electric devices such as dielectric condensers and varistors due to their properties of high dielectric constant, high dispersion frequency and small temperature dependence of the dielectric constant. The electric properties of these ceramic devices have been studied and found to be deeply influenced by the crystal growth mechanism, the grain boundary layer characteristics and the sintering atmosphere that is represented by such factors as oxygen partial pressure and processing temperature which relate to the atom vacancy formation. Atom vacancies, which play an important role to the electrical properties, have been detected by cathodoluminescence (CL) spectroscopy with scanning electron microscopy (SEM).

A ceramic condenser (Sr0.94Ca0.05Ba0.01)0.99TiO3 was investigated by Hitomi el at: using transmission electron microscopy (TEM). The material is a boundary layer (BL) semiconducting ceramic condenser, having dielectric layers between semiconducting grains. The same condenser material was investigated in this report at the grain boundary region using high resolution (scanning) transmission electron microscope (TEMSTEM) capable of High Angle Annular Dark Field (HAADF) technique.

Grain boundaries have long been known to have a deleterious effect on the superconducting critical current that can be carried by YBa2Cu3O7-δ. Recent theoretical analyses have proposed that the origin of this behavior may be band bending, which results in the depletion of charge carriers at the grain boundaries. For this to occur in these p-type superconductors there must, by definition, be a high density of localized donor states in the boundary plane. Here we describe a structural feature intrinsic to all [001] tilt boundaries that may be the origin of these localized states.

Direct atomic-resolution images of asymmetric [001] tilt grain boundary structures have been obtained using the Z-contrast imaging technique. The grain boundaries are observed to be composed of distinct structural units, as shown in figure 1. Within these structural units, a 2×1 reconstruction of the CuO columns is seen to occur. This reconstruction, which is caused by the constraint imposed on the structure by the sizes of the component atoms, leads to effective oxygen vacancies in the grain boundary plane (figure 2). Further oxygen annealing of the boundary cannot fill these vacancies as there is no space in the structure for more oxygen atoms.

In the last decade, Pd-Ge contact system emerged as the most promising replacement of the Au-Ni-Ge alloy, still used by most of today's GaAs technology. Its better electrical properties stem from the fact that contact formation is based on a series of solid state reactions without any melting of the metal thin films and the GaAs substrate taking place during annealing. Research studies by E.D. Marshall et al. (1) demonstrated that thermally stable contacts with low resistivities could be achieved by low temperature annealing of Pd and Ge thin films. Their studies also revealed that the excess Ge is regrown on top of the GaAs substrate by a solid state epitaxy mechanism.

Typical TEM cross-sectional specimen preparation techniques limit the electron transparent area and make the global characterization of the contact difficult. In this study, we employed a focus ion beam (FEB) method as described by Bassile et al.(2), which allowed us to observe a minimum of 4 microns of the interface cross section in each of the specimens examined.

Aluminum-magnesium alloys are currently being utilized in lightweight automotive components and their good strength and weldability characteristics has made them candidates for increased use. The primary problem with using aluminum alloys for automotive applications is their relatively low formability. Superplastic forming (SPF) is a viable method for producing high elongations and is enabled in these alloys by the manipulation of intermetallic particles (e.g. Al3Sc) that restrict grain growth at the high homologous temperatures necessary for this technique [1]. SPF of Al-Mg-Mn-Sc alloy has yielded elongations of over 600% [2]. However, Al3Sc particles age rapidly at high temperatures which can reduce their strengthening characteristics following deformation. It has been experimentally observed that the addition of Zr to Al-Sc alloys retards the aging of the Al3Sc precipitates [3]. This is beneficial for high temperature conditions like superplastic forming and welding. In this study we examine the location of Zr in the strupturc and how it may be inhibiting particle aging.