Internal reflection ellipsometry was used for detection of the consecutive coating of two polyelectrolytes, poly (allylamine hydrochloride) (PAH) and poly(acrylic acid) (PAA), onto a tantalum pentoxide (Ta(2)O(5)) substrate until the 10th bilayer. The UV patterned PAH-PAA-multilayer was characterized in air via ellipsometry and atomic force microscopy. Suited optical models enabled the determination of the layer thicknesses in wet and dry states. Linear multilayer formation could be proved by Attenuated Total Reflection - Fourier Transformed Infrared Spectroscopy measurements following the increase of the nu(C=O) band depending on the adsorption of the PAA. Streaming potential measurements after each layer deposition step indicated a change in surface charge after each layer deposition due to the consecutive coating of PAH and PM. In this article the internal reflection ellipsometry is shown to be a convenient possibility to analyze the modification of a thin transparent Ta(2)O(5) substrate. (C) 2011 Elsevier B.V. All rights reserved.