Layered titanates MLaTiO4 (M = Li, Na, K) powders were hydrothermally synthesized, derived from double hydrous oxides La2O3. 2TiO(2). nH(2)O in a basic medium. The formation conditions of these compounds with a pure phase were investigated. Details such as the structural and particulate properties of these powders were obtained from X-ray diffraction (XRD), IR spectroscopy, high-resolution electron microscopy (HREM), and other techniques.