Formation of plasmonically active silver, copper and composite silver-copper nanostructures were studied in this paper. Metallic nanostructures were fabricated by thermal disintegration, so called dewetting, of the thin films in an argon atmosphere. The formation process of the nanostructures was in-situ observed by a novel method, based on resistance measurements. The influence of the material and thickness of the initial thin film on temperature of their disintegration was investigated. Electrical measurements were validated by scanning electron microscopy observations, while metallic the behavior of nanostructures was studied by XPS method. The formation of silver-copper nanocomposite structures was confirmed by UV–vis spectroscopy. Plasmon resonance with two characteristic peaks for nanocomposite structures was observed.