Textural evolution and phase transformation in titania membranes: Part 1.—Unsupported membranes

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Abstract
Textural evolution in sol–gel derived nanostructured unsupported titania membranes has been studied using differential scanning calorimetry (DSC), differential thermal analysis (DTA), thermal gravimetry (TG), X-ray diffraction (XRD) and N2 adsorption. The anatase-to-rutile phase transformation kinetics were studied using the Avrami model. The precursor gel had a surface area of ca. 165 m2 g–1, which after heat treatment at 600 °C for 8 h reduced to zero. Undoped titania-gel layers transformed to more than 95% rutile after calcination at 600 °C for 8 h. The causes of surface-area reduction and pore growth were anatase crystallite growth and the enhanced sintering of rutile during transformation. Lanthanum oxide was identified as a suitable dopant for shifting the transformation temperature to ca. 850 °C. Lanthanum oxide doped titania showed an improved stability of porous texture compared to that of the undoped titania membranes.