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H2S plasma created by an electrode-less radio-frequency discharge was used to modify the surface properties of the polymer polyethylene terephthalate. X-ray photoelectron spectroscopy, secondary ion mass spectrometry and atomic force microscopy were used to determine the evolution of the surface functionalities and morphology. A very thin film of chemically bonded sulfur formed on the surface within the first 10 s of treatment, whereas treatment for more than 20 s caused deposition of higher quantities of unbonded sulfur. The sulfur concentration reached a maximum of between 40 and 80 s of plasma treatment; at longer treatment times, the unbonded sulfur vanished, indicating instability of the deposited sulfur layer. Large differences in the surface morphology were observed.