A detailed characterization of large-pore cagelike mesoporous SBA-16 silica materials with tailored
pore dimensions is reported. The materials were synthesized in a EO106PO70EO106 (F127)−butanol−H2O
system under mildly acidic conditions, and the pore diameters were tailored by varying the hydrothermal
treatment temperature. Structural information was acquired by full-profile analysis of powder X-ray
diffraction (XRD) patterns. High-resolution diffraction data were obtained for all the materials using
synchrotron radiation as the X-ray source, enabling a comprehensive XRD modeling supplemented with
the generation of electron density distribution maps. The structural parameters derived from the XRD
modeling were compared with data obtained from nitrogen and argon physisorption experiments performed
at −196 °C. An excellent agreement was found between the XRD modeling results and those obtained
by a new nonlocal density functional theory (NLDFT) kernel developed for pore size analysis based on
gas adsorption in spherical pores, while NLDFT analysis based on a cylindrical pore model was shown
to systematically underestimate the pore dimensions by about 30% which exceeds previous expectations.
Furthermore, the Barrett−Joyner−Halenda model was shown to give errors up to about 45% in the pore
size range above 4 nm. The structure of the surfactant−silica hybrid materials was also analyzed by
XRD, which shed more light on the structural changes accompanying the thermal surfactant removal
process. The present study is expected to provide a reference source for the accurate characterization of
large cagelike mesoporous silica materials, on the basis of a direct comparison of suitable data collected
independently by gas physisorption and comprehensive XRD modeling.