The conditions for the layer-by-layer synthesis by the method of the successive ionic layer deposition of Sn(IV)Mo(VI,V)(0.6)Oy(.)nH(2)O nanolayers on a silica surface were determined for the first time. The nanolayer thickness was controlled by the number of successive cycles. The composition and structure of these films were determined using Fourier transform infrared and UV/Vis transmission spectroscopy, X-ray photoelectron spectroscopy, X-ray difraction, and electron microprobe. It was found that under heating up to 200 degreesC, molecular water and hydroxyl groups are removed from the nanolayers, the bonds Mo-O-Mo and Sn-O-Mo are formed, and Mo(V) is oxidized to Mo(VI). (C) 2003 Elsevier Science B.V. All rights reserved.