Tunable mesoporous silica films were prepared though a sol-gel process directed by the self-assembly of various triblock copolymers. Positron annihilation γ-ray energy spectroscopy and positron annihilation lifetime spectroscopy (PALS) based on intense pulsed slow positron beams as well as ellipsometric porosimetry (EP) combined with heptane adsorption were utilized to characterize the open porosity/interconnectivity and pore size distribution for the prepared films. The consistency between the open porosities was examined by the variations of orthopositronium (o-Ps) 3γ annihilation fractions and the total adsorbed volumes of heptane. The average pore sizes deduced by PALS from the longest-lived o-Ps lifetimes are in good agreement with those by EP on the basis of the Barrett–Joyner–Halenda model, as indicated by a well fitted line of slope k = 1. The results indicate that the EP combined with heptane adsorption is a useful method with high sensitivity for calibrating the mesopore size in highly interconnected mesoporous films, whereas PALS is a novel, complementary tool for characterizing both closed and open pores in them.
In this paper, a series of mesoporous silica particles with different pore diameters were fabricated using tetraethyl orthosilicate (TEOS) as the network precursor, hexadecyl trimethyl ammonium bromide (CTAB) as a structure directing agent and 1,3,5-Trimethylbenzene (TMB) as a pore enlarge reagent. Compared with SAXRD and BET, the PALS may not only show the mesoporous information but also provide the structure information of microporous.
Mesoporous silica films on Si wafers were prepared via a sol-gel process using a triblock copolymer as the structural template. Spin-coated films were dried and subsequently subjected to Ar plasma treatments for decomposing the polymeric porogen. Mesopore formation in the silica film upon Ar plasma treatments was investigated by positron annihilation lifetime spectroscopy. In comparison with calcined silica film, much larger pores, more heterogeneous in size were found in silica film prepared with Ar plasma decomposition of the porogen.
Open Porosity and Pore Size Distribution of Mesoporous Silica Films Investigated by Positron Annihilation Lifetime Spectroscopy and Ellipsometric Porosimetry