The possibility of preparing NiO_1-x·zH₂O nanolayers on the silica surface by successive ionic layer deposition was demonstrated for the first time. Effects of the concentration and pH of reagent solutions and washing liquids, of the time of treating with them, and of the number of ionic layer deposition cycles on the kinetics of nanolayer growth were studied. Conditions were found for the formation of nanolayers by reactions of sorbed ions in a layer. The composition of the resulting layers was studied by the UV-Vis and IR Fourier spectroscopy and by chemical analysis. Their thickness was determined ellipsometrically. The synthesis yields layers of nickel peroxide compounds, their thickness being determined by the number of ionic layer deposition cycles at a level of nanometer fractions. Changes in the compositions of the nanolayers on keeping and heating in air were also studied.