The adsorption and in‐situ polymerization of monothiophene on Ag(111) has been studied by X‐ray photoemission (XPS), programmed thermal desorption (TDP) and mass spectrometry. Thiophene is physisorbed on Ag(111) and desorbs entirely below 250 K. Three different desorption peaks representing multilayers and two different monolayer states can be distinguished by TPD. X‐ray irradiation leads to polymerization in multilayers which is accelerated by enhanced substrate temperatures, whereas the polymerization process is quenched at the Ag surface.

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