Adsorption-induced
deformation of a series of silica samples with
hierarchical porosity has been studied by in situ small-angle neutron
scattering (SANS) and in situ dilatometry. Monolithic samples consisted
of a disordered macroporous network of struts formed by a 2D lattice
of hexagonally ordered cylindrical mesopores and disordered micropores
within the mesopore walls. Strain isotherms were obtained at the mesopore
level by analyzing the shift of the Bragg reflections from the ordered
mesopore lattice in SANS data. Thus, SANS essentially measured the
radial strain of the cylindrical mesopores including the volume changes
of the mesopore walls due to micropore deformation. A H2O/D2O adsorbate with net zero coherent neutron scattering
length density was employed in order to avoid apparent strain effects
due to intensity changes during pore filling. In contrast to SANS,
the strain isotherms obtained from in situ dilatometry result from
a combination of axial and radial mesopore deformation together with
micropore deformation. Strain data were quantitatively analyzed with
a theoretical model for micro-/mesopore deformation by combining information
from nitrogen and water adsorption isotherms to estimate the water–silica
interaction. It was shown that in situ SANS provides complementary
information to dilatometry and allows for a quantitative estimate
of the elastic properties of the mesopore walls from water adsorption.