| Summary: | It is demonstrated that UV (LED at 365 nm) irradiation with subsequent heating (90–110 °C) of the polystyrene matrix containing a soluble Au(I) compound ((Ph<sub>3</sub>P)Au(<i>n</i>-Bu)) results in the growth of gold nanoparticles within the sample bulk, as confirmed by UV-vis spectroscopy and TEM electron microscopy. Pure heating of the samples without previous UV irradiation does not provide gold nanoparticles, thereby facilitating optical image printing. Comparing the nanoparticles’ growth kinetics in samples with different precursor content suggests the nanoparticle growth mechanism through Au(I) autocatalytic reduction at the surface of a gold nanoparticle. Within the polymer matrix, this mechanism is suggested for the first time.
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