The results of synthesis of the vanadium oxide bronzes NaV2O5, K4.3V6O16.2, and Rb4.4V6O16.1 are presented. The synthesis process can be described by three steps: the 1st -production of the sol by dissolving the necessary materials in H2O2 solution, the 2nd -fabrication of the gel by heating up to 350 K, and the 3rd -heating up to 580-780 K for the water removal from the gel. The chemical composition of obtained bronzes was examined by using X-ray photoelectron spectroscopy (XPS) method.