Frontier areas of modern technology rely on the possibility to tailor surface properties such as wetting, adhesion, lubrication, corrosion, and biocompatibility on both microscopic and macroscopic scales. To a large extent, these options are provided by self-assembled monolayers (SAMs), which are 2D polycrystalline films of semi-rigid molecules that are chemically anchored to a suitable substrate. In addition, such layers represent a general platform for the arrangement of future molecular electronics devices, framework for Chemical Lithography, and a model system for macromolecular and biological assemblies. Synchrotron-based techniques represent a powerful tool box for the characterization of SAMs. A basic information on the chemical identity, integrity, molecular conformation and orientation in these films can be obtained by a combination of X-ray photoelectron and X-ray absorption spectroscopy (XPS and XAS, respectively). More specific questions, such as, e.g., bonding configuration of the anchor group or dynamics of the charge transfer along the molecular backbone require special experimental tools such as high-resolution XPS and resonant Auger electron spectroscopy, respectively. Using several model systems, we will illustrate application of the above techniques for the characterization of SAMs. In addition, we will show that SAM can be used as prototypes of highly organized biological systems and provide important implications for cryogenic approaches in advanced electron and x-ray microscopy and spectroscopy of biological macromolecules and cells.

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