For the first time the conditions of synthesis of Bi-V-O-containing nanolayers by the successive ionic layer deposition method were determined. The influence of synthesis conditions, such as the concentration and pH of the reactant solutions, time of treatment, and the number of ion-deposition cycles, on the kinetics of layer growth on a surface was studied. The deposited layers were studied by ellipsometry, UV-VIS and FT-IR spectroscopy, electron microprobe, and XRD methods. When BiOClO4 and NaVO3 are used as the reactants, the surface film with Bi/V ratio varying from 1:1 to 1:0.3 undergoes regular linear growth and its thickness can be controlled at a level of a nanometer and up. At pH approximate to 3, a nanolayer of BiVO4 is formed. The prepared layers were investigated after heating in air over the 100-500 degreesC range.