Very pure and crystalline ZrTiO4 microspheres (15-50 mu m) were prepared by two sol gel methods using a zirconia sol and two types of titania sols and characterized by scanning electron microscopy, X-ray diffraction and simultaneous differential thermal and thermogravimetric analysis. On gelation of the mixed sols, microspheres of an amorphous material with Zr/Ti ratio of similar to 1.0 were obtained by each route. The amorphous materials obtained by the two routes transformed to fully crystalline ZrTiO4 at 500 and 600 degrees C, respectively. The high temperature thermal stabilities of these materials were also studied.