title: Characterization of mesoporous thin films by specular reflectance porosimetry.
abstract: The pore size distribution of mesoporous thin films is herein investigated through a reliable and versatile technique coined specular reflectance porosimetry. This method is based on the analysis of the gradual shift of the optical response of a porous slab measured in quasi-normal reflection mode that occurs as the vapor pressure of a volatile liquid varies in a closed chamber. The fitting of the spectra collected at each vapor pressure is employed to calculate the volume of solvent contained in the interstitial sites and thus to obtain adsorption-desorption isotherms from which the pore size distribution and internal and external specific surface areas are extracted. This technique requires only a microscope operating in the visible range attached to a spectrophotometre. Its suitability to analyze films deposited onto arbitrary substrates, one of the main limitations of currently employed ellipsometric porosimetry and quartz balance techniques, is demonstrated. Two standard mesoporous materials, supramolecularly templated mesostructured films and packed nanoparticle layers, are employed to prove the concept proposed herein.
authors.affiliation: Instituto de Ciencia de Materiales de Sevilla, Consejo Superior de Investigaciones Científicas, Universidad de Sevilla, Sevilla, Spain.
authors.forename: Nuria
authors.initials: N
authors.lastname: Hidalgo
authors.forename: Carmen
authors.initials: C
authors.lastname: López-López
authors.forename: Gabriel
authors.initials: G
authors.lastname: Lozano
authors.forename: Mauricio E
authors.initials: ME
authors.lastname: Calvo
authors.forename: Hernán
authors.initials: H
authors.lastname: Míguez
mesh_terms: D010316:Particle Size; D016062:Porosity; D012822:Silicon Dioxide / Q000737:chemistry*; D013057:Spectrum Analysis / Q000295:instrumentation; D013499:Surface Properties; D014025:Titanium / Q000737:chemistry*
chemical_list: C009495:titanium dioxide; D012822:Silicon Dioxide; D014025:Titanium