Search

A model-based fitting algorithm for electron energy-loss spectroscopy spectra is introduced, along with an intuitive user-interface. As with Verbeeck & Van Aert, the measured spectrum, rather than the single scattering distribution, is fit over a wide range. An approximation is developed that allows for accurate modeling while maintaining linearity in the parameters that represent elemental composition. Also, a method is given for generating a model for the low-loss background that incorporates plural scattering. Operation of the user-interface is described to demonstrate the ease of use that allows even nonexpert users to quickly obtain elemental analysis results.

Electron coincidence spectroscopy in an ultrahigh vacuum scanning transmission electron microscope has been used to study the generation pathways for secondary (SE) and Auger electrons (AE) excited by high‐energy incident electrons. Energy and momentum transfer of inelastically scattered 100 keV primary electrons have been correlated with energy selected SE and AE for both thin 〈111〉 oriented Si crystals and amorphous C films. Coincidence spectra from the valence excitation region indicate that bulk plasmon decay is not the primary production channel for SE in Si(111) and that SE result partially from the decay of ionizations from deep in the valence band. Energy deposition by the primary beam is responsible for SE production at excitation energies above the valence region. At most one SE is emitted from the entrance surface of a thin film for each inelastically scattered 100 keV primary electron. An enhancement in both the SE yield and generation probability is observed at the C K ionization edge. Correl...

In recent years there has been a great upsurge of applications involving quantitative high-resolution electron microscopy, in particular comparing experimental micrographs with image simulations for determination of defect structures. Emphasis has been given to the determination of experimental parameters, the utilization of slow-scan CCD cameras for digital recording and extraction of quantitative structural and chemical information. More attention to surface cleanliness is needed to improve signal quality and the possibility of electron irradiation damage should not be overlooked. Issues related to adoption of a reliability of R -factor are briefly discussed.

The mean inner potential of a solid is a fundamental property of the material and depends on both composition and structure. By using cleaved crystal wedges of known angle, combined with dogital recording of off-axis electron holograms and with theoretical calculations of dynamical effects, the mean inner potential of Si (9.26±0.08 V), MgO (13.01±0.08 V), GaAs (14.53±0.17 V) and PbS (17.19±0.12 V) is measured with high accuracy of about 1%. Dynamical contributions to the phase of the transmitted beam are found by Bloch wave calculations to be less than 5% when the crystal wedges are titled away from zone-axis orientations and from major Kikuchi bands. The accuracy of the present method is a factor of 3 better than previously achieved by reflection high-energy electron diffraction and electron interferometry. The major causes of uncertainty were specimen imperfections and errors in phase measurement and magnification calibration.

The modern analytical transmission electron microscope gives signals from both elastically and inellastically scattered electrons at rates up to a few magabytes per second. A flexible multiasking system is needed to effectively integrate the information from a microscope with multiple detectors while synchronously controlling selected optical parameters of the instrument. We describe a system based on a Digital Equipment LSI-11 microcomputer equipped with a frame buffer and show how it has been used to develop new experimental capabilities such as time-resolved spectroscopy and multi-spectroscopy elemental mapping.

The optics of the illuminating system of a TEM/STEM equipped with a high-brightness field emission source has been studied in order to determine the current density distributions of small electron probes used for microanalysis. The experimental distributions were measured from high-magnification TEM images of the small probes, and compared to theoretical distributions calculated using both coherent and incoherent optics. The microscope was shown to be capable of producing an electron probe with a FWHM diameter of 1.7 nm and a current of 1 nA. The size of the probe is limited by electrical and mechanical instabilities.

Electron irradiation of maximally-valent transition-metal oxides within the transmission electron microscope leads to a variety of surface reactions which depend primarily upon the energy and local current density of the incident electron beam. When the oxides Nb 2 O 5 , V 2 O 5 , TiO 2 and WO 3 are irradiated at current densities of 5–50 A cm −2 then formation of the respective metallic monoxide is observed. The surface profile imaging technique reveals that the surface monoxide invariably has a well-defined epitaxial relationship with the original oxide. When a small focused probe of extreme current density (⋍10 3 -10 4 A cm −2 ) is used, reduction beyond the monoxide phase for WO 3 , V 2 O 5 and TiO 2 is observed. Extensive pitting, amorphization and some evidence for the based metal is also found. Measurements have also been performed under uhv conditions and show that sputtering from the exit surface is an important damage mechanism.

The effects of beam precession on the Electron Energy Loss Spectroscopy (EELS) signal of the carbon K edge in a 2 monolayer graphene sheet are studied. In a previous work, we demonstrated the use of precession to compensate for the channeling-induced reduction of EELS signal when in zone axis. In the case of graphene, no enhancement of EELS signal is found in the usual experimental conditions, as graphene is not thick enough to present channeling effects. Interestingly, though it is found that precession makes it possible to increase the collection angle, and, thus, the overall signal, without a loss of signal-to-background ratio.

This letter presents results of rapid processing for X-ray absorption correction in quantitative X-ray microanalysis using an analytical electron microscope. A computer-based system developed for analytical electron microscopy is used to assist in the extrapolation method, which does not require thickness measurement but only the recording of characteristic X-rays for absorption correction.

This study investigated the effects 2 h after administration of acetazolamide on cerebral blood flow and the pattern of cerebral capillary perfusion. Arterial blood pressure, heart rate, arterial blood gases, and pH were recorded in two groups of rats along with either regional cerebral blood flow or the percentage of capillary volume per cubic millimeter and number per square millimeter perfused as determined in cortical, thalamic, pontine, and medullary regions of the brain. Blood pressure, heart rate, and arterial PCO2 were not significantly different between the rats receiving acetazolamide (100 mg/kg) and the controls. Arterial blood pH was significantly lower in the acetazolamide rats. Blood flow increased significantly in the cortical (+ 102%), thalamic (+ 89%), and pontine (+ 88%) regions receiving acetazolamide. In control rats, approximately 60% of the capillaries were perfused in all of the examined regions. The percentage of capillaries per square millimeter perfused was significantly greater in the cortical (+ 52%), thalamic (+ 49%), and pontine (+ 47%) regions of acetazolamide rats compared with controls. In the medulla the increases in blood flow and percentage of capillaries perfused were not significant. Thus in the regions that acetazolamide increased cerebral blood flow, it also increased the percentage of capillaries perfused.

Electron holography, and high spatial resolution (17Å) computer controlled Parallel Electron Energy Loss Spectrometry (PEELS) were used to probe the structure of and chemical profile across a thin silicon Oxide-Nitride-Oxide (ONO) layered structure of nominal width 10Å-50Å-10Å. We found that the layer widths are on the average 13Å-28Å-18Å, the first oxide layer was discontinuous, and the second oxide layer contained nitrogen. The nitride layer had a silicon to nitrogen concentration ratio of 1.0 ± 0.1. These results show, for the first time, the power of holography in characterizing thin, light element, amorphous layers and the importance of computer controlled parallel energy loss line scans for obtaining analytical information at the highest spatial resolution with minimum dose.

Alterations in regional cerebral blood flow (rCBF) and percent perfused capillaries (indicative of functional intercapillary distance) were determined in conscious male Long-Evans rats after reducing their blood O2-carrying capacity by exposing them to 1% CO for 12 min. rCBF was determined by the iodoantipyrine method. rCBF increased from a mean of 106 +/- 8 (SE) ml.min-1.100 g-1 before CO exposure to 173 +/- 14 ml.min-1.100 g-1 after CO exposure. There was a greater flow increase (126%) in the cerebral cortex than in the lower brain stem [pons (45%), medulla (39%)]. Presence of fluorescein isothiocyanate-labeled dextran identified the perfused capillaries before and after CO exposure. The volume fraction (Vv) and number/mm2 (Na) of all capillaries (perfused and nonperfused) in a given area of brain were determined after staining for alkaline phosphatase. The percent Vv and percent Na of perfused capillaries increased uniformly (from approximately 50% to approximately 80%) in all parts of the brain after CO exposure. In the presence of tissue hypoxia with undiminished plasma PO2, the brain vasculature allowed greater flow of blood while the microvasculature adjusted to reduce the diffusion distance for O2.

Aluminum nitride is known to have a large affinity for oxygen as an impurity. At high levels (>∼4 wt/o) the oxygen is incorporated in the form of planar stacking faults where “pure” 2H AIN is regularly interspersed with a layer of oxygen at the faults. At oxygen levels lower than ∼ 4 wt/o the structure shows an expanded c-axis. The present authors have not observed this effect, rather a random distribution of stacking faults is observed along with another, more prevalent, extended defect identified as an inversion domain boundary (IDB). The IDBs are significantly aplanar (indicating a low interface energy), and often have precipitates and other, faceted defects associated with them. The role of these defects in oxygen accommodation in AIN has been investigated both structurally and chemically by electron optical methods (SEM, TEM, STEM, HREM, CBED, EDS, EELS, and CL-TEM). The structural nature of the boundaries, in the absence of oxygen, requires Al-Al or N-N bonding to occur with some frequency across the boundary. Such bonding is unlikely due to the excess energy required. Chemical analysis (EELS) and luminescence studies (CL-TEM) reveal that oxygen is often associated with the boundaries and may mediate the bonding at the boundary. A model is proposed for the IDB which includes structural aspects combined with considerations of stoichiometry in an effort to understand the origin and energetics of this defect.