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Nichtlineare Dynamik und PPS
(2001)
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.
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.