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  • PACS. 61.16.Bg Transmission, reflection and scanning electron microscopy (including EBIC) - 81.05.Tp Fullerenes and related materials; diamonds, graphite  (1)
  • Perovskite  (1)
  • 1
    ISSN: 1432-2021
    Keywords: Key words EELS ; Brownmillerite ; Perovskite ; TEM
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Notes: Abstract Observations by transmission electron microscopy (TEM) of the submicrometer phases present in calcium aluminate cements have shown that Ca-Al-Fe oxides coexist in two forms with brownmillerite (b) and perovskite (p) structures, respectively. Homogeneous single crystals of both brownmillerite and perovskite have been observed but exsolved lamellae also occur on the scale of tens of nanometers. Perovskite lamellae in brownmillerite exhibit coherent interfaces with an almost perfect [1 0 1]b = {1 0 0}p topotactic relationship. Energy-dispersive X-ray spectroscopy (EDXS) measurements show that perovskite lamellae are enriched in Ti and Si relative to the brownmillerite lamellae. The perovskite phase may accommodate up to 0.17 Si atoms per formula unit, but the exsolution process seems mainly to concern the Ti content. It is estimated that the solvus width ranges between concentrations of 0.06 〈 Ti 〈 0.13 atoms per formula unit. O K and Fe L 2,3 edges collected by electron energy loss spectrometry (EELS) confirm that both phases are mainly composed of Fe3+, requiring that the perovskite is highly oxygen-deficient. Al K and Si K EELS spectra have features comparable with those of fourfold-co-ordinated Al and Si sites, suggesting that they are probably located close to oxygen-vacant sites.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1434-6036
    Keywords: PACS. 61.16.Bg Transmission, reflection and scanning electron microscopy (including EBIC) - 81.05.Tp Fullerenes and related materials; diamonds, graphite
    Source: Springer Online Journal Archives 1860-2000
    Topics: Physics
    Notes: Abstract: Various filled carbon nanotubes have recently been successfully produced by the arc-discharge method by doping a 99.4% graphite anode with a transition metal like Cr, Ni, a rare earth like Yb, Dy, or a covalent element like S, Ge. In this work, the structural characteristics of these encapsulated nanowires were studied by High Resolution Transmission Electron Microscopy and their chemical composition was investigated using Electron Energy-Loss Spectroscopy with high spatial resolution: this analysis mode provides elemental concentration profiles across or along the filled nanotubes. Except in the case of Ge for which only pure Ge fillings were identified, surprising amounts of sulfur, which was present as an impurity ( 0.25%) in the graphite rods, were found within numerous filling materials. When using high purity carbon rods, no filled nanotube was obtained. We chose the case of Cr to clearly evidence that the addition of sulfur in catalytic quantity is responsible for the formation of filled nanotubes, including sulfur free encapsulated nanowires. A growth mechanism based on a catalytic process involving three elements, i.e. carbon, a metal and sulfur, and taking into account the experimental results is proposed.
    Type of Medium: Electronic Resource
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