The combination of focused ion beam (FIB) sample preparation and quantitati
ve electron spectroscopic imaging is an ideal toot for the investigation of
layered structures used in microelectronic metallization schemes. In the p
resent work, Si3N4/Cu/Si3N4/SiO2/Si and Al/TiN/Ti/SiO2/Si metallization lay
ers produced by physical vapour deposition are investigated. We apply serie
s of energy filtered images in the low loss region for a mapping of the sam
ple thickness which makes it possible to refine the parameters of the FIB p
rocess. We also show how series of energy filtered images in the core loss
region can be used to obtain elemental distribution images and chemical bon
ding information on these samples on a nanometre scale. For materials with
a small grain size and/or a strong variation in Bragg orientation, the inte
nsity distribution of the elemental map is strongly influenced by the super
imposed Bragg contrast. This detrimental effect can be reduced greatly by u
sing hollow cone illumination, as is demonstrated for polycrystalline Cu, O
ne striking feature observed in Cu layers prepared with FIB is strong, regu
larly arranged contrast variations caused by subsurface defects in the Cu g
rains, We suppose that these defects are a consequence of a strong interact
ion of Ga atoms from the FIB with Cu.