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In this work titanium sol was prepared from tetraethylorthotitanate (TEOT) in ethanol, stabilized with beta-diketonate 2,4 pentanedione in molar ratio 1:1 homogenized by magnetic stirring, europium ion was add as structural probe. The xerogels were heat treated at 500, 750 and 1000 °C and the characterization was realized by x-ray diffraction (XRD), transmission electron microscopy (TEM), thermogravimetric analysis (TGA/DSC) and photoluminescence (PL). The excitation spectra of Eu (III) ion present maximum in 394 nm correspondent to 5L6 level and emission spectra present bands characteristic transitions arising from the 5 D0 -> 7F J (J = 0, 1, 2, 3, 4) manifolds to samples treat at 500 and 750 °C. The Eu (III) emission disappear, when heated at 1000 °C, probably due to phase transition anatase to rutile and migrations of ions to the external surface that was proved by x-ray diffraction, transmission electronic microscopy and the thermogravimetric analyses of xerogels

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