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CuInS2 films are investigated with photoelectron spectroscopy. We find significant deviation from the stoichiometric composition depending on the preparation on the films. For Cu-rich films (start composition) we show that by Ar sputtering and annealing the surface composition varies along a binary cut of the Cu-In-S ternary phase diagram. We also present a novel technique which brings the surface composition close to the stoichiometric stability range of the CuInS2 phase. The technique used the evaporation of Cu on the sputter cleaned surface.
The composition of CuInS2-films tends to differ from the ideal ratio of 1:1:2. A molecularlyvariation of dm=[Cu]/[In]-1 not equal 0 occurs due to the formation of binary phases as segregation's at the surface, as crystallites in the bulk of the film or at the surface of grains [1]. Furthermore, the range of homogeneity of the phase CuInS2 is relatively large caused by a low enthalpy of formation of defects like Cu-vacancies [2]. Segregation's at surfaces can be removed by KCN etching or by an electrochemical process [3, 4] We investigated the effect of an in-situ-heat-treatment of samples, prepared in the Cu-rich regime with additional amounts of copper, deposited on the surface of the Cu-In-S-films.We used Cu-In-S-films on molybdenum, prepared from precursors of Cu/In and a following reactive annealing-process in a sulphur-atmosphere. The experiments were performed as follows: The surface of the films was cleaned in situ to remove CuS-Phases by Argon-bombardment. The thin layers of additional Copper were prepared by evaporation of copper metal in Knudsen-cells. The thickness of this copper-films is in the range of monolayers, revealed by a calibration with copper on iron-substrates. After this deposition the samples were heated up to several temperatures (up to 550 ºC) for ten minutes, respectively. Here the molybdenum back-contact was used as electrical heater.