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We applied the parametric bootstrap to the X-ray microanalysis of Si-Ge binary alloys, in order to assess the dependence of the Ge concentrations and the local film thickness, obtained by using previously described Monte Carlo methods, on the precision of the measured intensities. We show how it is possible by this method to determine the statistical errors associated with the quantitative analysis performed in sample regions of different composition and thickness, but by conducting only one measurement. We recommend the use of the bootstrap for a broad range of applications for quantitative microanalysis to estimate the precision of the final results and to compare the performances of different methods to each other. Finally, we exploited a test based on bootstrap confidence intervals to ascertain if, for given X-ray intensities, different values of the estimated composition in two points of the sample are indicative of an actual lack of homogeneity. [ABSTRACT FROM AUTHOR]

Qualitative and quantitative electron energy-loss spectroscopy analyses have been performed on niobium and stable niobium oxides (NbO, NbO2 and Nb2O5). At integration windows (Δ) greater than 75 eV, k-factor analysis can be used to distinguish between the stoichiometry of the three oxides within 5.7% error. As seen in other metal oxides, with increasing oxidation state the metal ionization edges shift to higher energies relative to the O-K edge. Normalized M2,3 white-line intensities show a strong correlation with 4 d occupancy for each compound. The data are in correspondence with that observed in the literature for 4 d transition metals using normalized L2,3 white lines. Lastly, a distinctive energy-loss near-edge, structure of the O-K edge was observed for each oxide, which could be used as a fingerprint for analysis of unknowns. [ABSTRACT FROM AUTHOR]

Summary Analytical electron microscopy was used to characterize aquatic iron-rich colloids. We focused our attention on a redox transition medium in the drainage water of a peat soil. In the anoxic peat water, observations by transmission electron microscopy and associated energy dispersive analyses (TEM-EDS) highlight the presence of spherical entities (∼100–600 nm), containing only traces of iron. The increase of dissolved oxygen concentration favours the formation of iron oxy(hydr)oxides. In the oxygenated drain, particles with the same morphology and size range are present. Statistical TEM-EDS analyses show that they represent the only colloidal form of iron in the drain samples. Nevertheless, although Fe–K peaks appear clearly on EDS spectra, the proportion of iron in these colloids reaches at most 4% at. (whereas C + O > 90% at.). Structural information completes this study. Both electron spectroscopic imaging (ESI) and electron energy-loss spectroscopy (EELS) reveal the disparity between element distributions within the drain entities. Iron and calcium are preferably distributed on the outer sphere of the particle, whereas carbon and oxygen follow the theoretical variation of the signal intensity within a plain sphere. The implication of organic matter as nucleation site for iron precipitation is spectacularly demonstrated by the presence of nanometre-sized iron-rich phases highlighted by EELS line scans. [ABSTRACT FROM AUTHOR]

Increasing the solid angle of X-ray collection is a major factor in improving the analytical sensitivity of X-ray energy-dispersive spectrometry (XEDS) in the analytical electron microscope (AEM). A new scanning transmission electron microscope, the VG HB 603, is equipped with two XEDS detectors with the largest collection angles (0.30 and 0.17 sr) available in commercial AEMs. However, large collection angles result in a large range of take-off angles, from ~ 4° to 36°, and the low angles can cause strong X-ray absorption. In order to investigate possible detrimental effects of the low (and of the range of) take-off angles on quantitative microanalysis of specimens exhibiting significant absorption, a stoichiometric Ni3Al thin-film, in which the Al Kα line is significantly absorbed, was analysed. Furthermore, the effect of different values of the collection angle on X-ray intensities was theoretically evaluated by numerical calculations and spectral simulation. These theoretical approaches permitted correlation of changes in the X-ray take-off angle (and hence X-ray absorption) with changes in the collection angle. It is demonstrated that ~ 0.30 sr detectors, with minimum take-off angles as small as 4°, only result in maximum errors of 4% in the quantification of Al in Ni3Al and, therefore, further increases in collection angle can be pursued while maintaining current levels of accuracy of quantification. [ABSTRACT FROM AUTHOR]

The interpretation of highly resolved elemental maps is not straightforward: one has to consider the quantum mechanical nature of the scattering process as well as the influence of the microscope. Existing calculations of the contrast in elemental maps are based on a non-relativistic approach, while in most of the currently installed electron microscopes, the electrons penetrate the specimen with relativistic energies ≥ 200 keV. Therefore, we have recalculated the intensity distribution in elemental maps based on a fully relativistic theory. Using the concept of contrast transfer functions, the simulations account for lens aberrations as well as the defocus. Surprisingly, the results exhibit considerable deviations between the relativistic and non-relativistic calculations even in the region of low acceleration voltages such as 100 kV. These differences increase with increasing acceleration voltage and are strongly dependent on aperture and energy loss. Quantitative simulations and evaluations of highly resolved elemental maps should therefore make use of a fully relativistic theory. [ABSTRACT FROM AUTHOR]

SUMMARY A new procedure has been developed to produce thin foils of uranium and its alloys for transmission electron microscopy. The procedure is a two-step electrochemical cleaning-thinning process which produces self-supporting discs. This procedure was used to produce thin foils of the most important alloys of uranium. [ABSTRACT FROM AUTHOR]