The first structurally characterised titanium and iron isopropoxide, [FeCl{Ti-2(OPri)(9)}] (1), has been used as a single-source precursor for TiO2/Fe2TiO5 Composites prepared by the sol-gel route. Two distinct hydrolysis and condensation conditions were employed, followed by drying and thermal treatment up to 1000 degreesC. Product composition and oxide phase transitions were characterised by powder X-ray diffractometry and Raman, electron paramagnetic resonance, Mossbauer and Fourier-transformed infrared spectroscopies. A mixture of nanometric-size TiO2 (anatase, 3.6-5.8 nm) and amorphous iron(III) oxide was obtained up to 500 degreesC, while TiO2 (rutile), alpha-Fe2O3 (hematite) and Fe2TiO5 (pseudobrookite) were found at 700 degreesC. At 1000 degreesC, only rutile and pseudobrookite were observed. These results suggest that 1 behaves as a type III single-source precursor. Powders calcined at 1000 degreesC were analysed for surface morphology, microstructure and elemental composition by scanning electron microscopy/energy dispersive X-ray spectroscopy. Results suggest no phase segregation on a sub-micrometer level. Different morphologies were observed for the materials produced by the N-2 route, and this could relate to early crystal growth in an oxygen-deficient environment. (C) 2003 Elsevier Ltd. All rights reserved.