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Dynamic determination of secondary electron emission using a calorimetric probe in a plasma immersion ion implantation experiment

A passive thermal probe has been used to detect dynamic changes in the secondary electron emission (SEE). Oxidized and nitrided materials have been studied during argon ion sputtering in a plasma immersion ion implantation process. Identical measurements have been performed for the metallic state with high voltage pulses accelerating nitrogen ions towards the surface, supposedly forming a nitride layer. Energy flux data were combined with scanning electron microscopy images of the surface to obtain information about the actual surface composition as well as trends and changes during the process. Within the measurements, a direct comparison of the SEE within both employed ion species (argon and nitrogen) is possible while an absolute quantification is still open. Additionally, the nominal composition of the investigated oxide and nitride layers does not always correspond to stoichiometric compounds. Nevertheless, the oxides showed a remarkably higher SEE compared to the pure metals, while an indistinct behavior was observed for the nitrides: some higher, some lower than the clean metal surfaces. For the aluminum alloy AlMg3 a complex time dependent evolution was observed with consecutive oxidation/sputtering cycles leading to a very rough surface with a diminished oxide layer, leading to an almost black surface of the metal and non-reproducible changes in the SEE. The presented method is a versatile technique for measuring dynamic changes of the surface for materials commonly used in PVD processes with a time resolution of about 1 min, e.g. magnetron sputtering or HiPIMS, where changes in the target or electrode composition are occurring but cannot be measured directly.