A. Fernandez et al., CHARACTERIZATION OF NANOPHASE AL-OXIDE AL POWDERS BY ELECTRON-ENERGY-LOSS SPECTROSCOPY, Journal of Microscopy, 191, 1998, pp. 212-220
Al nanoparticles were prepared by the inert gas condensation method. A
fter passivation with oxygen and air exposure we obtained a powdered s
ample of an Al-oxide/ Al nanocomposite material, In the present paper
we describe the use of the electron energy-loss spectroscopy (EELS) te
chnique in a transmission electron microscope to characterize such nan
ostructured powders compared with a microcrystalline commercial alumin
ium foil. Energy-filtered images showed the presence of an alumina ove
rlayer of = 4 nm covering the aluminium nanoparticles (23 nm in diamet
er), EELS analysis enabled us to determine the total amount of Al2O3 a
nd metallic Al and the structure of the alumina passivation overlayer
in the sample. Tn particular, the extended energy-loss fine structure
analysis of the data showed a major presence of Al tetrahedrally coord
inated with oxygen in the alumina passivation layer of Al nanoparticle
s instead of the octahedral coordination found for a conventional Al f
oil. This surprising effect has been attributed to the nanoscopic char
acter of the grains. The analysis of the electron-loss near-edge struc
ture also determines the presence of a certain degree of aggregation i
n this kind of powdered sample as result of the coalescence of the nan
ocrystalline grains. The procedure presented here may have the potenti
al to solve other problems during characterization of nanostructured m
aterials.