The use of nanoparticles has significantly increased in many areas, such as biomedical research, being highly useful as nanoprobes for imaging and as nanocarriers for drug delivery applications. Nevertheless, this potential can only be achieved with the correct characterization of the nanoparticles, since their size and shape can directly affect their biological behavior. \textcolor{red}{In this study, we propose a novel approach for a monolayer deposition of gold and platinum nanoparticles on Si substrates suitable for Medium Energy Ion Scattering (MEIS) analysis. The samples were prepared using PEG 6000 as a coating agent for the substrates, utilizing a spin coater—a versatile, cost-effective, and practical technique. The samples were first analyzed with the RBS technique to assess the adhesion and the overlapping of the nanoparticles in the substrates coated with PEG 6000 and then characterized through the MEIS technique.} The analysis through MEIS allowed the determination of the shape, size, and coverage area of the nanoparticles. Scanning and transmission electron microscopy were also performed on the samples, with the results corroborating the findings of the MEIS experiment. Together, the data obtained with microscopy and the MEIS technique suggests the effectiveness of the method in the production of monolayer samples.