Although conventional high-resolution transmission electron microscopy is a
powerful method for the elucidation of the structure of mesoporous solids
(diameter of pores from 1.5 to 20 nm), it is far less capable than high-res
olution scanning transmission electron microscopy in identifying the spatia
l distribution of nanocrystals of catalysts encapsulated within the mesopor
es. Using high-angle annular dark-field imaging (either in a 100 or 300 keV
STEM system), it is possible to locate precisely individual bimetallic nan
oparticles (Ag3Ru10, Cu4Ru12 and Pd6Ru6 hydrogenation catalysts) supported
on mesoporous silica, to determine their size distribution, and to record t
heir characteristic X-ray emission maps. It is also established that there
is little tendency for elemental fragmentation of the bimetallic catalysts,
all of which were prepared by decarbonylating, by thermolysis, precursor c
luster carbonylate anions: [Ag3Ru10C2(CO)(28)Cl](-), [Ru6C(CO)(16)Cu2Cl](2-
) and [Ru6Pd6(CO)(24)](2-).