Recently we have been investigating the mineralization of polymer-surfactant films to create thicker and more robust self-supporting membranes. Our previous experiments used the cationic surfactant-polyethylenimine system, and also mixtures of cationic and anionic surfactants with water soluble polymers. During SAXS studies on dried films we noticed that aging the polymer-surfactant template solutions at different temperatures has a marked effect on the size and type of nanostructure formed in the films. We therefore wish to investigate the structures in these films at the air-solution interface and to use selective deuteration of the surfactants to determine whether the thermal history affects the molar ratio of the two species in the films. We will study both silica and titania films since these have a wider range of potential applications in catalysis and photoelectrochemical devices.