Zirconium titanate powders were synthesized by a straightforward sol–gel method using zirconium and titanium chlorides as metal precursors, deionized water as solvent and oxygen donor, and a NaOH solution for adjusting pH to 7. According to transmission electron microscopy, amorphous particles of nearly 5nm in size with a relatively spherical morphology were prepared. Thermogravimetry and differential scanning calorimetery analyses on the xerogel at a heating rate of 10°C/min indicated a crystallization temperature of 690°C, which is comparable with previous reports. Furthermore, via differential scanning calorimetery studies using the Kissinger's equation, the activation energy for ZrTiO 4 crystallization was determined to be 850kJ/mol. Structural evaluations in the isothermal regime, using X-ray diffraction experiments, implied the onset of ZrTiO 4 crystallization at 550°C.