Mesoporous thin film architectures
are an important class of materials that exhibit unique properties,
which include high surface area, versatile surface functionalization,
and bicontinuous percolation paths through a broad library of pore
arrangements on the 10 nm length scale. Although porosimetry of bulk
materials via sorption techniques is common practice, the characterization
of thin mesoporous films with small sample volumes remains a challenge.
A range of techniques are geared toward providing information over
pore morphology, pore size distribution, surface area and overall
porosity, but none of them offers a holistic evaluation and results
are at times inconsistent. In this work, we present a tutorial overview
for the reliable structural characterization of mesoporous films.
Three model samples with variable pore size and porosity prepared
by block copolymer (BCP) coassembly serve for a rational comparison.
Various techniques are assessed side-by-side, including scanning electron
microscopy (SEM), atomic force microscopy (AFM), grazing incidence
small-angle X-ray scattering (GISAXS), and ellipsometric porosimetry
(EP). We critically discuss advantages and limitations of each technique
and provide guidelines for reliable implementation.