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Solid state devices based on copper indium diselenide, (CIS), have produced world record efficiencies for polycrystalline photovoltaic solar cells. In order to understand thin film phase transformations that are relevant to the production of CIS, multilayer thin films of copper and indium have been analyzed. Using differential scanning calorimetry, X-ray diffraction, scanning electron microscopy, and X-ray photoelectron spectroscopy, the reaction pathways for equal atomic concentration, copper rich, and indium rich films were established. Indium was found to react during deposition, so that the as-deposited films consisted of CuIn2 and copper. During constant heat rate experiments, the excess concentration of copper within the film provided the driving force in the formation of phases richer in copper. The Cu11In9 phase was observed to form from CuIn2 and Cu at 130 °C, and Cu7In3 formed from Cu11In9 and Cu at 310 °C. In the indium rich samples, a given phase was found to be stable until melting. In films with an overall indium concentration exceeding the concentration of Cu11In9, the excess indium was shown to move primarily to the film surface, and in indium rich films, to grain boundaries between the Cu11In9 phase.

The details of the sulfurization reaction of Cu/In metallic precursor layers for the preparation of CuInS2 photovoltaic absorbers have been investigated. For this, an experiment has been designed in order to establish the main mechanisms that govern the sulfurization reaction. A metallic layer containing Cu and In (Cu/In = 1.8) has been processed using a combined sequence of sulfurization and selenization steps. Afterwards, this sample was investigated by Auger electron spectroscopy, Raman spectroscopy, and transmission electron microscopy in order to study its microstructure and chemical composition. The results show that the sulfurization reaction of these films is dominated by the out-diffusion of the metallic atoms through the chalcogen layer. Moreover, taking into account our previous investigations we have developed a consistent model for the formation of these absorber layers.

We investigate Cu-In thin films used as precursors for the production of CuInS2 and Se2 solar-cell absorber material via reactive annealing. The films are produced by coevaporation of Cu and In onto glass substrates and are characterized by means of Rutherford backscattering and x-ray diffraction (XRD). The interplay of phase composition, morphology, and surface topography is studied as a function of chemical composition, substrate temperature, and annealing processes. The analysis of the XRD data is based on known crystallographic data for the phases Cu7In3 (δ-phase), Cu16In9 (η'-phase), Cu11In9, and In. Refined crystallographic data for CuIn2 are presented, and the low-temperature modification of Cu16In9 (η-phase) is investigated by means of bulk powder samples. These data and the inclusion of texture effects allow us to perform a complete RIETVELD type analysis of the Cu-In precursors. It is shown that, in contrast to sequentially evaporated films, all known Cu-In equilibrium phases can be formed during film deposition. These are Cu7In3, Cu16In9, Cu11In9, and CuIn2. Moreover, it is found that single-phase films of all these phases can be produced. Film roughness is shown to increase with deposition temperature and In content. The results presented offer new prospects for sulfurization and selenization processes in solar-cell production.

CuInSe2 films of various stoichiometries have been prepared by the two-stage process. In this method, Cu-In layers were first evaporated onto Mo-coated glass substrates in the form of stacks, and then they were selenized in a H2Se atmosphere at 400 °C to form the compound. CdZnS/CuInSe2 heterojunction solar cells were fabricated on these films and conversion efficiencies close to 7% were obtained.

Abstract CuInSe2 films have been prepared using the selenization technique. Preparation of the precursor as well as selenization were carried out by the vacuum evaporation technique. The sequence of copper and Indium layer deposition during precursor preparation affects the morphological and structural properties of precursor which directly have effects on the properties of selenized CIS films. A thin layer of amorphous selenium at the substrate/film interface has been used to improve the adherence of the film. The effect of the Se under-layer has been studied on the layers of copper, indium, CuIn precursors and CIS films, using structural, morphological and optical properties. The surface morphology of a single layer of copper and indium, with and without the Selenium under-layer, are quite different and drastically affect the properties of the precursor and selenized films. The Se under-layer does not take part in the chemical reaction of CIS formation during the selenization process. The modified CIS films are uniform, single phase, polycrystalline, chalcopyrite with (1 1 2) preferred orientation showing an energy band gap of 0.99 eV and an absorption coefficient of ~10^5 cm-1, and have good adherence to the substrate for the scotch tape test.

CuInS2 films were synthesized by sulphurization of In/Cu stacked elemental layers (SEL) deposited onto glass and Mo-coated glass substrates by graphite box annealing at temperatures of 620-880 K. The films thus synthesized were characterized by measuring electrical, optical, microstructural and photoluminescence properties. The microstructure and hence the physical properties of the films depended critically on the amount of sulphur incorporation. Nature of charge carriers depended on both Cu/In and S/(Cu+In) ratio and the carrier concentration varied between 10^14 and 10^18 cm^-3. Grain boundary scattering effects were critically studied by measuring the electrical conductivity and Hall mobility simultaneously on the same sample. The shape of the grains depended critically on the sulphur content. The PL spectra were dominated by the excitonic peak ~788 nm followed by another peak at ~892 nm which may be ascribed to the DA transition.