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This work pursues a novel route to functionalizing large surfaces with hybrid nanoparticles. It also casts new light on the combined use of surface plasmon resonance and X-rays. SPR spectroscopy is employed to study Au-based plasmonic nanostructures fabricated by novel methods, and a new experimental device is developed combining SPR with X-ray absorption spectroscopy at a synchrotron beamline. Using the new SPR-XAS setup developed in this work, the author has studied in-situ and real-time effects of X-ray irradiation in materials such as glasses and Co-phthalocyanines.