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The structure of the nanocrystals was examined by X\u2010ray diffraction, UV\u2010vis ground state diffuse reflectance absorption spectra and X\u2010ray photoelectron emission spectroscopy. Results showed that samples prepared by sol\u2013gel process and calcined at 400 \u00b0C are composed of a mixture of anatase and rutile phases, in contrast to the one prepared by solid\u2010state sintering, which exhibits an anatase phase with Li being involved in a spinel phase. The photocatalytic degradation of aqueous solutions of different aromatic compounds was successfully achieved under sunlight excitation in presence of Li\u2010doped TiO<jats:sub>2<\/jats:sub> prepared via sol\u2013gel process. It was shown that the calcination temperature and the preparation mode greatly affect the photocatalytic efficiency. 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