The crystal shape of Ni particles, dewetted in the solid state on sapphire substrates, was examined as a function of the partial pressure of oxygen (P(O2)) and iron content using scanning and transmission electron microscopy. The chemical composition of the surface was characterized by atom-probe tomography. Unlike other FCC equilibrium crystal shapes, the Ni crystals containing little or no impurities exhibited a facetted shape, indicating large surface anisotropy. In addition to the {111}, {100} and {110} facets, which are usually present in the equilibrium crystal shape of FCC metals, high index facets were identified such as {135} and {138} at low P(O2), and {012} and {013} at higher P(O2). The presence of iron altered the crystal shape into a truncated sphere with only facets parallel to denser planes. The issue of particle equilibration is discussed specifically for the case of solid-state dewetting.
SummaryTransmission electron microscopy specimens in the form of elongated, conical needles were made using a dual-beam focused ion beam system, allowing the specimen thickness to be geometrically determined for a range of thickness values. From the same samples electron energy loss maps were acquired and the plasmon mean free path (λ) for inelastic scattering was determined experimentally from the measured values of specimen thickness. To test the method λ was determined for Ni (174 ± 17 nm), α-Al 2 O 3 (143 ± 14 nm), Si (199 ± 20 nm) and amorphous SiO 2 (238 ± 12 nm), and compared both to experimental values of λ taken from the literature and to calculated values. The calculated values of λ significantly underestimate the true sample thickness for high accelerating voltages (300 kV) and large collection angles. A linear dependence of λ on thickness was confirmed for t/λ < 0.5-0.6, but this method also provides an approach for calibrating λ at sample thicknesses for which multiple scattering occurs, thus expanding the thickness range over which electron energy loss spectroscopy can be used to determine the absolute sample thickness (t/λ > 0.6). The experimental method proposed in this contribution offers a means to calibrate λ for any type of material or phase that can be milled using a focused ion beam system.
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