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Fe, Co, and Ni magnetic nanoparticles have been characterized
using energy-selected imaging in a high-resolution transmission
electron microscope. The samples comprised Fe/FeOx
and Co/CoOx nanoparticles synthesized by inert gas
evaporation and a Ni/C nano-composite prepared by a sonochemical method.
All of the particles examined were found to be between 5 and
30 nm in size, with the Fe and Co crystals coated in 5–10
nm of metal oxide layer and the Ni metallic crystallites embedded
in an amorphous carbon spherical matrix.
Electron Tomography is shown to be applicable to problems of materials science if a contrast mechanism is used which provides a projection relationship for crystals not depending on lattice plane orientation. Energy filtered TEM (EFTEM) in its mode of electron spectroscopic imaging (ESI) and STEM-EDX-Mapping are, subject to limitations, suitable image formation techniques. The spectroscopic operation not only allows to overcome Bragg scattering artefacts, but offers the possibility of recording 4-dimensional data (volume and energy) of a region of interest, otherwise only known from NMR and XAS/XANES tomography at larger length-scales and from field-ion microscopy (atom probe) under restrictive conditions.
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