Strengthening mechanism of porous silica films derived by two-step catalysis

A scratch-resistant improvement of sol-gel derived nano-porous silica films by a base/acid two-step catalysis is reported. The silica films were prepared with the two-step catalytic sol-gel process and a dip-coating method, and then post annealed in air and a mixed gas atmosphere. The films were characterized with FE-SEM, AFM, TEM, XPS, FTIR, an ellipsometer, and an abrasion test. With the post annealing, the frequency shift of the FTIR absorption ω4(TO3) peak of the films to a lower wavenumber results from a decrease in the average Si-O-Si bridging angle. An increase in the full-width at half-maximum of the ω4 peak is ascribed to a wide distribution of the bridging angle because of formation of strained Si-O-Si bonds caused by the post annealing. XPS analysis shows that the effect of the mixed gas annealing on the binding energy and full-width at half-maximum (FWHM) for Si (2p) and O (1s) peaks is attributed to the further condensation reaction of the films resulting from the disappearance of the OH groups. The abrasion and adhesion tests indicate that the two-step catalysis obviously improves the scratch resistance and adhesion of the films, and that the mixed gas treatment further strengthens the silica network. The increase in strength is attributed to more Si-O-Si bond cross-linkages between silica particles formed by the two-step catalysis and the mixed gas treatment.