Z-contrast images and electron energy loss spectra (EELS) were obtained from low angle grain boundaries in SrTiO3 and YBa2Cu3O7-x (YBCO). Z-contrast images are easy to interpret and especially useful for positioning the beam to acquire EELS data from small sample areas [1], because both these techniques can be performed simultaneously.

In high-temperature superconductors even a single grain boundary can reduce the critical current by up to four orders of magnitude. The band-bending model can quantitatively explain this phenomenon. YBCO is a hole-doped superconductor with about one hole per unit cell for optimum doping at x close to zero. It has a structure closely related to the perovskite structure, and Z-contrast images have shown that the dislocation cores are made up of similar structural units as in SrTiO3.[2,3] Our EELS measurements show clear evidence for band bending effects around isolated dislocation cores in an undoped 8° low angle grain boundary.

The properties of ceramic oxides being developed for such varied applications as fuel cells, ionic transporting membranes, high-Tc superconductors, ferroelectrics and varistors are dominated by the presence of grain boundaries. Key to controlling the electronic properties of the grain boundaries in these materials is a fundamental understanding of the complex relationship between structure, composition and local electronic structure. The ability to characterize and directly correlate these parameters on the atomic scale is afforded by the combination of Z-contrast imaging and electron energy loss spectroscopy (EELS) in the scanning transmission electron microscope (STEM). Furthermore, the recent development of in-situ heating capabilities in the JEOL 201 OF STEM/TEM permits atomic resolution analysis to be performed at elevated temperatures and the interactions of grain boundaries with the oxygen vacancies determined.

Figure 1 shows an example of the type of experiment that can be performed using these methods.

High resolution transmission electron microscopy (HREM) is an excellent experimental method to image grain boundary structures with atomic resolution. The advantage of the method is the short exposure time of only about one second that is needed to record an image. Other methods like Z-contrast imaging require much longer exposure times and are therefore much more prone to specimen drift during recording. However there is the remaining difficulty to HREM that the evaluation of experimental images is not straightforward and a thorough analysis of the images is necessary in order to deduce quantitative information with small error bars of only a few pm (10-15m). A second inherent difficulty common to all atomic resolution imaging techniques is that the information is retrieved from a very small area of a specimen. The question arising from that is: can we nevertheless be sure to obtain a representative answer to a “real world” material science problem? A positive answer to this question is given by the investigations presented here.

Extended structural defects in α-Al2O3 (alumina), a technologically important, complex ceramic material were quantitatively analyzed with respect to grain boundary segregation, atomic and electronic structures using spatially resolved electron energy-loss spectroscopy (EELS), energy dispersive X-ray spectroscopy (EDS) and first-principles local-density-functional (LDFT) calculations. in this study the results of analytical investigations will be compared with the outcome of LDFT calculations.

The analytical measurements were performed with a dedicated scanning transmission electron microscope (TEM) VG HB501UX, operating at 100 kV and with a typical beam diameter of lnm. For the spatially resolved EELS a parallel electron energy-loss spectrometer (Gatan model 666) with an energy resolution of better than 0.8 eV was used. For the chemical analysis an EDS system (Noran-Gresham with a Si(Li) detector and a Norvar window) was applied. The detection limit of the EDX system for measuring interface excess is in the range of 0.3 atoms/nm2.

A variety of semiconductor and metal nanoparticles can be synthesized and tunable in size from about 10 to 200 Å using size-selective separation technique. Preparation of monodisperse samples enables systematic characterization of the structural, electron, and optical properties of materials as they evolve from molecular to bulk in the nanometer size range. Sample uniformity makes it possible to manipulate nanocrystals into close-packed, glassy and ordered nanocrystal. At inter-particle separations 5-100 Å, dipole-dipole interactions lead to energy transfer between neighboring nanocrystals, and electronic tunneling between proximal nanocrystals gives rise to dark and photoconductivity. The fabrication of monodisperse ordered nanoarrays with the inter-particle separations less than 5Å will be very important to study its physical properties since interaction between neighboring nanocrystals cause otherwise insulating assemblies to become semiconducting, metallic, or superconducting depending on nanocrystals composition. Here we present the fabrication of monodisperse PbSe nanoarrays with inter-particle distance less than 5 Å and its nanostructure study.

Patterned nanostructures and nanodots are attracting increasing interest in the information storage industry. The ultimate recording density of a magnetic medium will have single domain dots aligned in arrays and each dot in such an array acts as a recording bit. The ideal structure is that the dots are magnetic and the surrounding medium is non-magnetic so that each dot can switch magnetization direction freely without the interference from other dots. This paper presents the nanostructure of the nano-dot array investigated by transmission electron microscopy and magnetic force microscopy. The Co:C film was deposited by alternatively sputtering Co target and C target. The as-deposited specimen has an amorphous structure as revealed by electron diffraction in TEM. Such films transform to ferro-magnetic ones after heat treatment [1]. A laser beam of wavelength of 308 nm and a flux of 0.24 J/cm2 was split into two beams of an approximately equal intensity and then recombined, generating an interference pattern and a periodic modulation of the light intensity.

The growth of self-organized nanoislands and nanowires on a substrate has been extensively studied with a view to fabricating the new functional materials and advanced electric devices. in the present work, Pd silicide islands and wires grown on Si (111) 7x77×7surface were observed in situ by ultrahigh vacuum transmission and reflection electron microscopy (UHV-TEM/REM). Pd was deposited on Si (111) 7×7 surface at about 700 K using an electron beam evaporator attached to the column of a UHV microscope. Two kinds of specimens were prepared: a <111> oriented rectangular specimen with a thin area, whose (111) top surface was observed by plan viewed TEM, and a <110> oriented bulk rectangular specimen, whose (111) side surface was observed by REM

Figure la shows a REM image of Si (111) 7×7 surface. An incident electron beam is directed from the top to the bottom of the figure, which is foreshortened in the beam direction.

Y2O3 is a super refractory oxide with high thermal stability and finds various applications in optics and microelectronic devices. Recently, Eu-activated Y2O3 films attracted much research interest due to its promising applications in flat panel field emission displays. Epitaxial Y2O3:Eu thin films have been grown on LaA1O3(LAO). in this paper we report a transmission electron microscopy (TEM) study of Y2O3 nano tip-structure grown on LAO by pulsed laser deposition using stoichiometric YBa2Cu3O7-σ.a target under a low oxygen pressure. The experimental work was conducted within a JEOL2010F TEM equipped with an ED AX system.

Fig.l is a low magnification cross-section TEM image of the nano-tip structure grown on (001) LAO. The lattice parameters of the tips were calculated to be that of Y2O3 by using LAO as a standard for indexing the diffraction patterns. Nano electron beam diffraction patterns from the tips along [100] and [110] axis are shown in Fig.2a and Fig.2b, respectively, in agreement with the simulated ones using bulk Y2O3 structure.

Molybdenum-based alloys possess a unique combination of physical properties including high strength at elevated temperatures, high thermal conductivity, low coefficient of thermal expansion, and excellent performance in neutron flux environments. However, welds in commercial grade molybdenum alloys typically exhibit low (∼3%) ductility which limits their application. Bryhan has shown that controlled additions of substitutional and interstitial alloying elements can provide almost 20% elongation from gas-tungsten arc welds in 6.35-mm-thick material. Therefore, molybdenum alloys may be considered for use in fusion reactors and other high temperature applications.

The molybdenum alloy was vacuum arc-cast with 0.16 at % Zr intended to getter the O (250 appm) and N (178 appm) impurities together with 53 appm B and 96 appm C intended to strengthen the grain boundaries. The 4-pass welding process was performed on a 6.35-mm plate in a controlled atmosphere chamber where the O, N and water vapor impurity levels were < 10 wppm each.

Interfacial anisotropy complicates the prediction of microstructural evolution, particularly ir extreme cases for which the presence of facets and corners prevents the application of classical notions of grain-boundary curvature. Although there has been much effort at incorporating anisotropic grain-boundary properties, including faceted geometries, into computational approaches for microstructural evolution, at present our mechanistic understanding of the behavior of facets anc their junctions remains limited. In this presentation, we investigate the development of faceted boundaries between Σ=3 <111> oriented grains in epitaxially deposited gold thin films. This system is well suited tc experimental studies of facet evolution since the crystallography and structure of the boundaries is already well understood. It is well known that “double-positioning” of epitaxially aligned <111> grains on a surface of three-fold or six-fold symmetry results in a microstructure composed of grains in two twin-related (Σ=3) variants that are separated by facets running vertically through the film and forming 120 degree corners [1,2].

Grain boundary migration (GBM) during the sintering and densification of a polycrystalline ceramic material occurs as a result of mass transport across an interface. When there is a liquid film present, either due to additives used for liquid-phase sintering or unavoidable impurities in the material, the mass transport can be visualized in terms of dissolving material from one grain and precipitating it on another. in order to study the effects of crystallography on GBM in the presence of a liquid phase, alumina bicrystals have been fabricated with anorthite (CaA12Si208) glass films at the interface. The alumina-anorthite system in a bicrystal geometry is used because the pseudo-binary phase diagram of the system is well known, the bicrystal geometry allows for control over the original interface misorientation, and the glassy phase of anorthite is the most commonly occurring glass in commercially used alumina.

Fig. 1 is a secondary-electron SEM image of an alumina bicrystal recorded using a field-emission SEM (Hitachi S900) operating at 5 kV.

We have used High Velocity Oxy-Fuel (HVOF) thermal spray coating process to obtain tungsten carbide coatings on steel. It is important to control the powder quality and surface roughness of the substrate in the thermal spray coating process to obtain good adherence. The adhesive strength is greatly effected by the interfacial impurities. Most commonly used in the thermal spray industry is Al2O3 grit abrasive for good surface roughness of steel substrate to produce anchor patterns for the coating. The previous studies indicated that some fine Al2O3 particles are trapped in the rough surface grooves during this process. The ring shear test method, described previously, appears to give the most accurate results on shear adhesive strength. The ring shear strength test was comprised of a 0.02” thick and 0.25” wide ring coating on a 1” diameter cylindrical substrate rod. This rod is placed in a disk with a cylindrical hole of the rod size and an incremental pressure is applied on the rod.

Interest in wide band gap III-V nitride semiconductor devices is increasing for optoelectronic and microelectronic device applications. to ensure the highest quality, TEM analysis can characterize the substrate and buffer layer interface. Measurements taken by TEM reveal the density of dislocations/cm2 and the orientation of Burger's vectors. This information allows for changes to be made in deposition rates, temperatures, gas flow rates, and other parameters during the processing.

The GaN/sapphire samples grown at AFRL were produced in two consecutive steps, first to provide a thin buffer layer, and the other to grow a lum thick epitaxial film. Both growth steps were prepared using metallic organic chemical vapor deposition (MOCVD) in a vertical reactor. Buffer layers were prepared using a range of temperatures from 525 to 535°C and with a range of flow rates and pressures in order to optimize the nucleation conditions for the epitaxial films.

Nonorthogonal twinings have commonly been observed in perovskite oxides such as SrTi03 and BaTi03. Among them, the ﹛111﹜ Σ3 type twining exists with a relative large amount of population and has been extensively studied. By combining quantitative high resolution transmission electron microscopy (HRTEM) and spatially resolved electron energy loss spectroscopy (EELS), one was able to determine the atomic structure of the ﹛111﹜Σ3 twin boundary in these oxides.[l] On the other hand, nonorthogonal twinings in SrRuO3 have been much less studied. SrRu03, a ternary ruthenium metal oxide, has a perovskite-compatible structure and exhibits low electrical resistivity (10-4 Ω•cm), showing an unparallel technique importance in microelectronic applications. Since the properties of material strongly depend on the microstructure and defect configurations, it is important to study the twining structures and their formation mechanisms in SrRuO3 thin films.

Transmission electron microscopy (TEM) was used to study the SrRuO3 thin films grown on (001) LaAlO3 by 90° off-axis rf sputtering.

Multilayers, heterostructures, nanostructures and composites are of great interest to the materials scientists, and frequently we encounter crystals lacking centrosymmetry. Thus crystal polarity determination on a microscopic scale is becoming increasingly important in describing interface structures and the internal defects in small crystals. in many cases the polarity of a crystallite can be determined by convergent beam electron diffraction, CBED. Powerful alternatives are to monitor the electron induced x-ray emission, EDS, or electron energy losses, EELS, under channeling conditions. While the determination of the phase of the structure factors, and thus the determination of the crystal polarity, relies on many beam diffraction effects when the CBED technique is used, two-beam experiments provide information about the phase of the structure factor when localized EDS or EELS signals are detected under channeling conditions.

The experimental conditions used to determine the polarity and absolute orientation from electron channeling are similar to those used in ALCHEMI experiments to locate small amounts of atoms by electron channeling.

Transparent conductive oxide materials (TCO) are currently under development for use as electrodes in devices such as photovoltaics and flat panel displays. As electrode area increases in large-area applications (e.g. photovoltaics), the resistivity of the TCO must decrease in order to maintain efficiency. The ideal next generation TCO will be a low cost material with a substantially higher conductivity than ITO obtained by improving mobility. Two promising TCO's are CdIn2O2 and Cd2SnO4 which both exhibit high conductivities (4300 S/cm and 8300 S/cm, respectively) and high mobilities (44 and 60 cm2/Vs, respectively).

A bulk investigation of the system CdIn2O4 - Cd2SnO4 reveals a large spinel solid solution, Cd1+xIn2.2xSnxO4 (0<x<0.75) at 1175°C exhibiting a sharp decrease in measured optical gap (from 3.0 to 2.8 eV) at x=0.2 and an increase in conductivity (from 2200 S/cm to 3500 S/cm) for reduced specimens between x=0.4 and x=0.60) with increasing x. It is suspected that the cation distribution (e.g. normal, random, or inverse) on the spinel lattice may be important in understanding these shifts in electrical and optical properties.

Atom location by channeling-enhanced microanalysis (ALCHEMI) promises a straightforward measurement of ordering in materials. On tilting the electron beam in a transmission electron microscope (TEM) about a superlattice Bragg position the electron channeling changes, weighting X-ray production from each of the sublattices differently. The overall X-ray signal, converted to an apparent composition via a kinematical non-channeling standardization, moves between the composition of the constitute sublattices. However, the accuracy of measurement always bothers many researchers. Results may vary from time to time, and in the worse cases, the composition outputs are nonsense. Table 1 gives an example of a series of ALCHEMIC measurements in a B2 Ti50Al42Mo8 intermetallic alloy.

In general, two major sources cause errors in ALCHEMI: weak channeling and delocalization effects. The later only results in “systematic errors”, which can always be corrected or reduced by theoretical calculations. However, it is difficult to improve the error due to weak channeling.

Quantitative analysis in the TEM by EELS or EDXS depends on the K-factor method in which uniform ionization, independent of specimen orientation and thickness, is assumed. This assumption is of limited validity for crystals, where channeling of the electron wave ψ affects the ionization rate as observed in both energy loss and X-ray signals. Both EELS and EDXS are sensitive to changes in ψψ*near the atomic sites, and this variation as a function of crystal orientation forms the basis for ALCHEMI. Simultaneously recorded EELS and EDXS spectra were used to monitor changes in Cu/Ba ratio from YBaCu-oxides using L2,3/M4,5 ionization edges or K/L X-rays respectively. Although the acceptance aperture for EELS (11 mrad at 300 keV) may not be sufficiently large to mask double-channeling effects, it is small enough that momentum transfer is sufficiently limited to enhance derealization. Thus it is expected that the EELS signal should be less sensitive to crystal orientation than EDXS (an estimate of impact parameters yields 0.73 and 0.61 Å for the Ba and Cu energy loss signals, reducing to 0.06 and 0.04 Å respectively for X-ray emissions).

Introduction:Atomically resolved chemical analysis using techniques such as electron energy loss spectroscopy and annular dark field imaging relies on the ability to form a well-characterised sub-nm electron beam in a FEGTEM/STEM [1-2]. to understand EELS+EDX-signal formation upon propagation of a sub-nm beam through materials we first have to assess precisely the beam intensity distribution in vacuum and find conditions for the best obtainable resolution.

Experimental Details:Modern TEM/STEM instruments combine features of both imaging and scanning technology. The beam forming capability approaches closely that for dedicated STEMs, while CCD recording devices allow us to measure the beam profile by direct imaging at magnifications up to 1.5 M. The recording of a “z-section” series through the 3D intensity distribution of the cross-over can therefore be realised by recording of a “condenser focal series”.

Nickel-base superalloys (NBSAs) have remarkable mechanical properties (and corrosion resistance) at elevated temperatures. Single crystal NBSAs have found major use as turbine blades in aeroengines, where there is a large world market because the turbine blades have to be replaced at regular intervals. in order to develop engines with higher efficiency, considerable efforts are being devoted to enhance the temperature capabilities of superalloys. The two phase γ-γ’ structure that is crucial to NBSA characteristics is primarily produced by the presence of Al in combination with Ni: above a critical concentration the Ll2 γ’ phase based on Ni3Al precipitates out of the γ Ni-base solution. However, superalloys usually contain many other alloying elements such as Cr, Co, Mo, W and Ta to enhance strength and impart higher temperature performance. Among these alloying additions, much attention has recently been paid to Re because of its contribution to the improvement of both creep and corrosion properties.