Gold nanocrystallites dispersed in an inhomogeneous gold matrix are detected by high-resolution scanning electron microscopy using a field emission source and backscattered electron detection in the composition mode, as well as by energy-filtered transmission electron microscopy in the plasmon energy region. The identity of the nanocrystalline domains was established by observing the same evaporated gold film samples but using bright-field, dark-field, electron diffractogram, and electron energy loss spectroscopy images in the transmission electron microscope. Comparison of these images shows that backscattered electron and plasmon energy detection can be used to identify crystalline domains in an otherwise chemically uniform sample. (C) 2001 Academic Press.235148