According to the different phases at which titanium dioxide (TiO2) crystallizes, previous studies have shown that anatase is more efficient for photocatalysis than rutile. Nowadays, the synergetic effect is well-accepted between anatase and rutile as having an effect in increasing performance in photocatalysis. In the present work, control over the anatase/rutile ratio was performed in three experimental steps. Initially, amorphous-anatase TiO2 powders were synthesized by the sol-gel method. For the crystallization of anatase, the powders were annealed at 250 °C for 2 h in ambient atmosphere. The final step was performed by using different annealing times, ranging from 35 up to 200 min at a temperature of 475 °C. The powders were characterized by Raman spectroscopy, UV–VIS, SEM and TEM techniques to determine the crystalline phase, band gap, morphology, and elemental composition, respectively. It was possible to control the anatase/rutile ratio on the nanostructured TiO2 powders from 100% of anatase until a complete transformation to rutile through the variation of the annealing time. The band gap calculated using the Tauc’s model was found in the range of 2.56 to 2.93 eV. However, no direct relationship between the anatase/rutile ratio, and the band gap was found.
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