In Situ Monitoring Mesoscopic Deformation of Nanostructured Porous Titania Films Caused by Water Ingression

Nanostructured porous titania films are used in many energy-related applications. In this work, the temporal evolution of the mesoscopic deformation of mesoporous titania films synthesized via block copolymer-assisted sol-gel chemistry is investigated with in situ grazing incidence small-angle neutron scattering (GISANS) during exposure to D₂O vapor. Two types of mesoporous titania films are compared, which have a different degree of structural stability, depending on the applied annealing temperature (400 °C vs 600 °C) in a nitrogen atmosphere. Water ingression causes a gradual structure deformation in terms of decreasing center-to-center distances and broadening of the size distribution of the titania nanostructures. Based on the evolution of the mesopore size obtained from in situ GISANS measurements, the results show that structures synthesized at lower temperature undergo a stronger deformation because of the lower elastic modulus originating from larger pores, despite having a higher degree of order.