In this paper, the results of XPS and AFM studies of the surface chemistry and morphology of In2O3 nanolayers obtained by rheotaxial growth and vacuum oxidation (RGVO) technology are presented. The ultrathin In films were deposited under UHV by thermal evaporation of indium pellets on the well defined Si substrate maintained at different temperatures. Optimal conditions to obtain the smallest grains and highest surface coverage have been determined, which was controlled by AFM, whereas the cleanness of deposited In nanolayers was controlled by XPS method. The ultrathin films of In2O3 (nm scale) were obtained in two ways, i.e. by oxidation of ultrathin films of In after their deposition, as well as by oxidation of In ultrathin films already during the deposition process. The XPS experiments showed that in both cases the obtained ultrathin films of In2O3 were almost stoichiometric. In turn, the AFM studies confirmed that only ultrathin films obtained during the simultaneous In deposition and oxidation exhibit almost flat surface morphology with average roughness at the level of about 0.85 nm. (C) 2011 Elsevier B.V. All rights reserved.