Conjugated polymer-based organic photovoltaic devices (OPVs) have been intensively studied, since they are advantageous over regular inorganic devices. However, there is still no complete understanding of the functionality of conjugated polymer-based organic active layers. Due to this, research into the processes of microstructure formation will improve morphology control and optimization and enhance performance and productivity. In this study we used in situ measurements of conductivity and X-ray diffraction analysis in grazing incidence X-ray diffraction (GIXD) geometry to investigate the structure of light-sensitive layers produced by coating from solutions and based on poly(3-hexylthiophene) (P3HT) mixtures as donors with various fullerene acceptors: [6,6]-phenyl-C61 butyric acid methyl ester (PCBM) and indene-C60 bisadduct (ICBA). The structure of films produced by coating from solutions was studied by large-angle GIXD. Ex situ and in situ methods (under external voltage applied) were used to detect high compatibility between the donor and acceptor for ICBA-based films. The time dependences of changes in current and intensity of the (100) peak of P3HT demonstrate that the maximum emerges simultaneously. A two-step increase in intensity of the (100) peak of P3HT was observed for films containing PCBM as an acceptor. In situ studies of the structure confirm that the joint donor-acceptor structure is formed as the solvent evaporates. Atomic force microscopy studies of the surface roughness of films containing different acceptors demonstrate that they are characterized by different morphologies.Keywords: organic photovoltaic devices, in situ studies of the structure and electric properties, X-ray diffraction in grazing incidence X-ray diffraction geometry, polymer crystallization.

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