Abstract: The growth features of FeCr2S4 spinel single crystals prepared by chemical vapour transport were studied by means of scanning electron microscopy, transmission electron microscopy, high resolution electron microscopy, electron diffraction and X-ray analysis. Our results indicate that the epitaxial growth of the new phases FeCr7S12 and FeCr8S12, both based on the NiAs structure, can essentially inhibit the growth of large FeCr2S4 spinel single crystals in the octahedral habit. The new phases are fully characterised and the effects of defect ordering in these new phases are also reported.

Abstract: The structure of the metastable Ni2Al phase, which has long been a matter of controversy, has been carefully re-examined by means of high-resolution transmission electron microscopy (HREM) and electron microdiffraction. First, it is concluded that theas-quenched NixAl100-x(60 less-than-or-equal-to x less-than-or-equal-to 65) material already exhibits a partial omega-type collapse in a one-dimensional fashion which and is consistent with the anomalous dip in the phonon dispersion curve. Ni2Al precipitates are formed on annealing by thermal decomposition of the high-temperature NixAl100-xB2 phase and still retain the small omega-type shuffle. The amount of displacement in the well developed Ni2Al phase was estimated to be between 20 and 50% of the ideal omega collapse; this was determined by means of a combined technique of HREM and microdiffraction together with dynamical calculations of HREM images and diffraction intensities.

Abstract: Correlated noise is generally present in experimentally recorded electron energy loss spectra due to a non-ideal electron detector. In this contribution we describe a method to experimentally measure the noise properties of the detector as well as the consequences it has for model-based quantification using maximum likelihood. The effect of the correlated noise on the maximum likelihood fitting results can be shown to be negligible for the estimated (co)variance of the parameters while an experimentally obtained scaling factor is required to correct the likelihood ratio test for the reduction of noise power with frequency. Both effects are derived theoretically under a set of approximations and tested for a range of signal-to-noise values using numerical experiments. Finally, an experimental example shows that the correction for correlated noise is essential and should always be included in the fitting procedure. (c) 2007 Elsevier B.V. All rights reserved.

Abstract: The effect of temperature on the structural, electronic and optical properties of dense tetrahedral amorphous carbon made of similar to 80% sp(3)-bonded atoms is investigated using a combination of the classical Monte Carlo technique and density functional theory. A structural transformation accompanied by a slight decrease of the sp(3) fraction is evidenced above a temperature of about 600 degrees C. A structural analysis in combination with energy-loss near-edge structure calculations shows that beyond this temperature, the sp(2)-bonded C sites arrange themselves so as to enhance the conjugation of the p electrons. The Tauc optical band gap deduced from the calculated dielectric function shows major changes beyond this temperature in accordance with experimental results. Energy-loss near-edge structure and band gap calculations additionally reveal a massive destabilization of the of sp(3) bonding phase in favour of sp(2) bonding at a temperature of about 1300 degrees C which agrees very well with the reported value of 1100 degrees C.