We report the preparation of nanocrystalline anatase and rutile TiO(2) from aqueous peroxotitanium complex (PTC) solutions and their characterization by powder X-ray diffraction (XRD), infrared spectroscopy, and Raman spectroscopy. The phase evolution of TiO(2) prepared using PTC derived from different precursors, i.e., TiCl(4) and titanium tetraisopropoxide (TTIP), is related to the nature of the intermediate steps. Phase-pure nanoanatase was formed in PTC solution derived from TiCl(4), while a mixture of minor anatase and dominant rutile were prepared from PTC when TTIP was used as precursor. On the other hand, in the case of calcining PTC powders in air, a pure anatase phase of TiO(2) was obtained, regardless of the precursor used. Thus, the formation and attachment of hydrated TiO(6) units or TiO(2)·xH(2)O under a different environment, especially pH, plays a critical role in determining the phase during the crystallization of TiO(2).
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