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Dynamics of Crystallization and Disorder during Annealing of P3HT/PCBM Bulk Heterojunctions

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School of Physics and Astronomy, Cardiff University, Queens Buildings, The Parade, Cardiff CF243AA, United Kingdom
Department of Physics and Centre for Plastic Electronics, Blackett Laboratory, Imperial College London, Prince Consort Road, London SW7 2BW, United Kingdom
*E-mail: [email protected]. Tel: +44 (0)29 2087 0162 (lab). Fax: +44 (0)29 2087 4056.
Cite this: Macromolecules 2011, 44, 8, 2725–2734
Publication Date (Web):March 16, 2011
Copyright © 2011 American Chemical Society

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    A real-time crystallographic analysis of P3HT/PCBM films during thermal annealing is reported, detailing the temporal variation of crystallization, disorder, and orientational spread during the annealing. Five P3HT/PCBM chlorobenzene solutions with different P3HT concentrations (0, 33, 50, 67, 100 wt %) were spin coated on SiO2 substrates. The thick films (∼100 nm) were studied during annealing (50 min at 140 °C), with in situ synchrotron grazing incidence X-ray diffraction (GI-XRD) and a sampling time <8 s. For the first time, the evolution of the crystal structure is analyzed taking into account P3HT paracrystallinity. The following were observed: a predominance of edge-on P3HT lamellae in the as-spun and annealed films; changes in concentration-dependent edge-on lamellar orientation spread along the alkyl-stacking direction and paracrystalline disorder after annealing; a permanent lamellar stretching just along the alky-stacking direction after annealing; an increase in the P3HT domain size along only the alkyl-stacking direction for the edge-on lamellae, with dynamics consistent with PCBM acting as a plasticizer for P3HT; and finally, an increase in the PCBM concentration at the sample−air interface. We show that the paracrystalline correction is important to calculate correctly the domain size as deduced from GI-XRD.

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    Experimental details; data analysis (calibration equations, sample−detector distance, conversion pixels q values, out-of-plane line profiles, remarks on P0x, P0y accuracy, line profiles extraction, line profiles fitting); refraction correction; paracrystalline disorder; results (P3HT nanowires, d spacing vs αi, d spacings vs time and annealing temperature); five videos showing 390 images from in situ annealing of P3HT/PCBM films of different compositions; and a video showing the flattening of Δqh002/(2π)2 versus n4 due to the annealing. This material is available free of charge via the Internet at

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