Quantitative elemental mapping by inner shell core-loss energy-filtered transmission electron microscopy (TEM) with a Gatan Imaging Filter (GIF) interfaced to a Philips CM30 TEM operated with a LaB6 filament at 300 kV has been applied to interfaces in a range of materials. Typically, 15s exposures, slit width Δ = 30 eV, TEM magnifications ∼2000 to 5000×, and probe currents ≥200 nA, were used. Net core-loss maps were produced by AE−r background extrapolation from two pre-edge windows. Zero-loss I0 (Δ ≈ 5 eV) and “total” intensity IT (unfiltered, no slit) images were used to produce maps of t/λ = ln(IT/I0), where λ is the total inelastic mean free path. Core-loss images were corrected for diffraction contrast by normalization with low-loss images recorded with the same slit width, and for changes in thickness by normalization with t/λ, maps. Such corrected images have intensities proportional to the concentration in atoms per unit volume. Jump-ratio images (post-edge divided by pre-edge) were also produced. Spectrum lines across planar interfaces were recorded with TEM illumination by operating the GIF in the spectroscopy mode with an area-selecting slit oriented normal to the energy-dispersion direction. Planar interfaces were oriented normal to the area-selecting slit with a specimen rotation holder.
Anomalously Large Formula Unit Volume and Its Effect on the Thermal Behavior of LiBF4
