Nanosized metal particles embedded in glass have attracted much interest as material with potential applications because of their specific linear and non-linear optical properties. Especially, strong variations of the properties are expected for particle sizes much less than 10 nm. Therefore, we investigated the formation of very small Ag nanoparticles of 1 to 2 nm size in commercial soda-lime glass, silver-doped by Ag/Na ion exchange in a mixed nitrate melt such that Ag⁺ were incorporated into the glass replacing Na⁺ of the matrix. It could be shown by electron paramagnetic resonance and X-ray absorption spectroscopy that at the Fe K-edge that polyvalent Fe ions served as thermosensitive reductive during the ion exchange below the glass transformation temperature. This process could be described by a charge transfer between the iron ions and nuclei of Ag particles. The transmission electron microscopy, the optical spectroscopy as well as the X-ray absorption spectroscopy at the Ag K-edge were used to identify the formation of metal particles and to analyse the their structure. For sizes from 0.5 to 2 nm the experimental data indicate the presence of Ag containing structures (like oxidic compounds) that obviously serve as predeccessor for the formation of silver nanoparticles. The extensive analysis of the kinetics reveal that all previous models fail, in particular for nucleation and particle growth. It is assumed, that a new model must be established considering metastable intermediate phases in order to explain all experimental results.

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