Preparing highly dispersed monoatomic Cu species on a TiO2(110) surface was successfully achieved on a TiO2(110) surface that had been precovered with an acetic anhydride layer. Polarization-dependent total reflection fluorescence X-ray absorption. ne structure (PTRF-XAFS) spectra indicated that the three-dimensional structures of the monoatomic Cu species were stabilized on the surface by two 0.196-nm-long C-O bonds, namely, Cu-O (acetate) and Cu-O (bridging surface oxygen) bonds. The Cu species diffusion was effectively blocked by the acetate species with its molecular plane perpendicular to the [001] diffusion direction created by the dissociative adsorption of acetic anhydride. (C) 2009 Elsevier B.V. All rights reserved.