The formation of titanium oxide monolayer coatings on silica surfaces

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The formation of a dispersed titanium oxide layer on Cabosil-fumed silica and on nonporous silica spheres was studied by infrared and Raman spectroscopies and by transmission electron microscopy (TEM). The procedure for obtaining the titania coatings involved reacting the silanol groups on the silica surface with titanium alkoxides under a N 2 atmosphere. This self-limiting reaction led to a coating of dispersed titania on the silica spheres with a weight loading between 0.5 and 1.4 × 10 −3 g/m 2. The dispersed titanium oxide on the silica spheres was visible as a surface texturing of the silica in TEM images, and led to over two orders of magnitude increase in the reactivity of the silica spheres for 1-propanol dehydration. Raman spectroscopy and TEM confirmed that the dispersed titania was stable to calcination in dry air at 973 K or to heating under a vacuum of 2 × 10 −7 Torr up to 1058 K. However, under alcohol dehydration reaction conditions, the dispersed titania transformed into crystals of anatase, 3 nm in diameter. On Cabosil-fumed silica, on the other hand, a similar preparation resulted in a titania loading (per square meter) that was only 7% of that seen on the silica spheres. Higher loadings caused the appearance of bands due to crystalline TiO 2 (anatase) in the Raman spectra. The lower monolayer capacity on Cabosil silica can be correlated with the presence of singly bound hydroxyls as seen by IR. The Stober spheres on the other hand show hydroxyl bands that show significant hydrogen bonding.