CuInSe2 and related chalcopyrite compounds are the most promising absorber materials for polycrystalline thin film solar cells. CuInSe2 solar cells have shown the highest conversion efficiencies of all thin film solar cells. The record efficiency is 18.8 %, and several groups have achieved efficiencies over 18 %. Further, the operational lifetimes of this type of solar cells are long due to their extraordinary stability. CuInSe2 thin films can be prepared both from gas and liquid phases by a variety of methods, but the highest efficiencies have so far been obtained by absorbers prepared by co-evaporation. In order to lower the production costs of photovoltaic modules, alternative, low-cost deposition methods need to be developed. Electrodeposition is one alternative since it is a low-temperature liquid phase deposition method. The deposition equipment is relatively simple, and the advantages of the method include the potential for upscaling to large substrate areas and production volumes.
Electrodeposited CIS-based absorber films require generally annealing either under a Se-containing or an inert atmosphere prior to the cell preparation. Such approaches have resulted in conversion efficiencies between about 5 and 7 %. Even higher efficiencies, over 15.4 %, can be achieved if the stoichiometry of the electrodeposited precursor film is adjusted by adding In, Ga and Se by PVD prior to the cell preparation.
CIS-based films have been prepared by a variety of electrochemical techniques such as one-step deposition, sequential deposition of binary compounds, and deposition of elemental layers followed by annealing either under an inert or a reactive atmosphere. One-step electrodeposition is the most widely studied option. There are basically two alternative ways to control the film composition: either by balancing the diffusion fluxes of the constituent ions to the cathode, or by relying on thermodynamics. In the former case, the film composition is heavily dependent on the deposition potential and on the concentrations in the deposition solution. Small, unavoidable variations in concentrations and deposition potentials may therefore result in large changes in the film compositions which deteriorates reproducibility and may render upscaling to larger substrate areas problematic.
The latter option, in turn, utilizes induced co-deposition that has been used widely for binary compounds, especially CdTe. In a binary system, the deposition of the more noble ion induces the underpotential reduction of the less noble ion and the formation of the compound at less negative potentials than where the less noble ion would reduce on its own. The reason for the underpotential reduction of the less noble ion is the energy released in the compound formation.
When the deposition solution contains a large excess of the less noble ion, induced co-deposition ensures the formation of stoichiometric compound over wide concentration and potential ranges.
These kind of processes are thus much less sensitive to electrolyte composition and deposition potential than those based on the flux balance approach.
Despite its success in deposition of binary compounds, induced co-deposition had not been utilized for the deposition of ternary compound semiconductors prior to this work. In the case of CIS, this is partly because the formation of CIS occurs via Cu2-xSe, and the latter does not follow the induced mechanism. In the present work, suitable conditions for the induced co-deposition of Cu2-xSe and CuInSe2 were achieved by complexing the Cu+ ions by thiocyanate ions in order to shift the reduction potential of metallic Cu to the negative direction. Under these conditions, Se reduced first, i.e., at more positive potentials than Cu. The reduction of Se induced the formation of Cu2-xSe at more positive potentials than where the bulk deposition of metallic Cu began. Cu2-xSe, in turn, induced the formation of CuInSe2 at the same potential range, i.e., at more positive potentials than where the deposition of metallic Cu or In began. The electrochemistry of the Cu-Se and Cu-In-Se systems was studied by cyclic voltammetry and electrochemical quartz crystal microbalance measurements that verified the deposition mechanisms. Induced co-deposition allowed wide potential and concentration ranges for the formation of almost stoichiometric CuInSe2 films (Cu1.30In1.00Se2.20 according to RBS) as long as the concentrations of the metal precursors were much higher than that of the selenium precursor, and the concentration of the SCN- ions was high enough to keep all the Cu+ ions as [Cu(SCN)4]3- so that there were no free Cu+ ions in the solution.
The films were studied by a number of techniques: XRD, SEM, EDX, RBS, TOF-ERDA, photoelectrochemical and capacitance-voltage measurements. The as-deposited films were amorphous and contained hydrogen, oxygen, sulfur, carbon, and nitrogen as impurities. Hydrogen and oxygen originated apparently from the aqueous deposition solution and the other impurities from the thiocyanate ligands. The films became crystalline upon annealing that also reduced the impurity contents drastically. The relative amounts of Cu, In, and Se in the films remained essentially the same after annealing.
Since photovoltaic-quality CIS films should be Cu-deficient rather than Cu-rich like the films deposited in this study, two approaches were made to adjust the film compositions after deposition: etching in KCN solutions and addition of In2Se3. The effects of the post-deposition treatments on the film properties were studied by EDX, photoelectrochemical and capacitance measurements that verified more stoichiometric composition and more suitable carrier concentrations after the post-deposition treatments. However, the carrier concentration was still much higher than those measured for high-efficiency absorbers.
Solar cells were prepared from films deposited and treated under the conditions bound to give the highest photoactivities and lowest carrier concentrations. Doped ZnO films for the devices were prepared either electrochemically, by ALD, or by sputtering. For the first time, Al and In doped ZnO films were prepared by electrodeposition. The electrodeposited ZnO films were prepared from solutions containing Zn(NO3)2 and Al(NO3)3 or InCl3. The films were crystalline as deposited but did not result in good photoresponses due to their high resistivity. The
current-voltage characteristics measured in the dark showed, however, good rectifying behavior. This was also the first time when electrodeposited ZnO:Al and ZnO:In films were used as front electrodes in solar cells.
The photoresponses with the ALD-ZnO films were better than with the electrodeposited ZnO films. Yet, the best photoresponses were obtained from the devices with sputtered ZnO bilayers, prepared at HMI Berlin. The highest conversion efficiency, measured under AM 1.5 illumination, was 1.3 %. Although the efficiency was low, the open circuit voltages of these devices were comparable to those of higher efficiency devices with electrodeposited CIS absorbers.
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