Nanocrystalline mesostructured porous titania thin films with optimized coating and thermal curingconditions have been prepared for the first time using spin-coating deposition technique. The X-raydiffraction (XRD) and the grazing incidence small-angle X-ray scattering (GI-SAXS) measurementsrevealed that the crystallization and diffuse sintering of amorphous TiO
2 into anatase are simultaneouslystarting between 400 and 500
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C curing temperature, leading to a gridlike open-pore-shape transformation.The environmental ellipsometric porosimetry (EEP) measurements show that the 550
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C-cured TiO
2films exhibit a high porous volume (0.30 cm
3 g
-1), a large surface area (172 m
2 cm
-3), and a Youngmodulus of 1.05 GPa. All solid-state dye-sensitized solar cells (DSSC) based on nanocrystallinemesostructured TiO
2 films and poly(3-octylthiophene) as hole conductor allow reproducible achievementof energy conversion efficiencies of about 0.52%. These values, obtained with thin TiO
2 films (250 nm),are very promising.