The lithiated transition metal oxide LiVMoO6 has been synthesized by a novel melt quenching method that presents some advantages as compared to the classical solid-state reaction and soft-combustion synthesis. These are: the short preparation time and the possibility to control the grain size of LiVMoO6 powders. The local structure of LiVMoO6 samples prepared in different ways was characterized by IR spectral analysis. The oxidation state of Li, V, and Mo was determined by X-ray photoelectron spectroscopy.