Self-assembled or grafted onto organic monolayer on the solid surface of a solid-liquid interface can have the role of a sensing layer in biosensors or a protective layer in tribology processes or lab-on-chip systems. Therefore, studying the organization and the behavior of these layers in different environments is very important in order to further understand the application in which they are used. The purpose of our study is the characterization of these interfaces by force spectroscopy, or 1D-AFM, and 3D-AFM [1], [2]. In particular, we are interested in gold-thiol layer-liquid interfaces for biosensing and tribological applications [3]. Four samples were used: pure gold, pure Poly(Acrylic Acid) PAA, pure Poly(Ethylene Glycol) PEG, and 50/50 PAA/PEO. We measured these samples in pure water and in a 0.01M PBS solution. The shifts in the frequency Δf recorded during the 3D-AFM scan were used in a Python program to create a 2D (xz) color coded cross-sectional image of the scanned samples. Our first experiments tend to show that this 3D-AFM method is appropriate to visualize the difference in behavior between the samples caused by different polymer chain-tip interactions during the measurement. [1] T. Fukuma, R. Garcia, ACS Nano, 2018, 12, 11785-11797. [2] H. Asakawa, S. Yoshioka, K. Nishimura, T. Fukuma, ACS Nano, 2012, 6, 9013-9020. [3] M. F. Delcroix, G. L. Huet, T. Conard, S. Demoustier-Champagne, F. E. Du Prez, J. Landoulsi and C. C. Dupont-Gillain Biomacromolecules, 2013, 14 (1), 215–225.