Mesostructured composite materials, with features ranging from 20 to 500 An
gstrom in size, are obtained by the kinetically controlled competitive asse
mbly of organic and inorganic species into nanostructured domains. Short-ra
nge order is limited, and long-range order is determined by weak forces suc
h as van der Waals or hydrogen-bonding. Three-dimensional mesoporous materi
als obtained by removing the organic phase are of particular interest for a
pplications such as catalysis and chemical sensing or separation, for which
structural features such as cavity shape, connectivity and ordered bimodal
porosity are critical. But atomic-scale structural characterization by the
usual diffraction techniques is challenging for these partially ordered ma
terials because of the difficulty in obtaining large (>10 mum) single cryst
als, and because large repeat spacings cause diffraction intensities to fal
l off rapidly with scattering angle so that only limited small-angle data a
re available. Here we present a general approach for the direct determinati
on of three-dimensional mesoporous structures by electron microscopy. The s
tructure solutions are obtained uniquely without pre-assumed models or para
metrization. We report high-resolution details of cage and pore structures
of periodically ordered mesoporous materials(1,2), which reveal a highly or
dered dual micro- and mesoscale pore structure.