Poly(3-hexylthiophene) (P3HT) and 6,6-phenyl-C60 butyric acid methyl ester (PCBM) are model materials used to study and understand the performance of polymer solar cells. A critical design parameter in improving device performance is the structural morphology of the active layer. Traditional processing of organic solar cells involves the deposition of a P3HT/PCBM composite film from a common solvent and then post-processing treatments (i.e. annealing) to influence the extent of phase segregation and improve the percolation of electron and hole transport pathways throughout the film volume. Therefore, the electronic properties of the resulting solar cells are inherently tied to how the film is processed (e.g. choice of solvent, annealing temperature, film thickness). While process optimization has led to improvements in laboratory performance, it is challenging to extend the same principles to improve the performance of large scale roll-to-roll processes because deposition conditions vary significantly. Increasingly, researchers recognize the need for methods that decouple film processing from active layer structure and device performance. My research involves the synthesis of P3HT/PCBM composite nanoparticles (CNPs) in aqueous dispersion as a means to circumvent the dependence of active layer structure on the specific mode of deposition of the P3HT/PCBM film. I have synthesized CNPs with variable content of P3HT/PCBM and different preparation procedures while also controlling particle size. The characterization of these particles focuses on spectroscopy, small angle X-ray scattering (SAXS), dynamic light scattering and the performance evaluation of devices produced with CNP active layers. This project will tie device performance to CNP structure regardless of active layer processing, and assist in identifying CNPs with optimized morphology without the need for annealing or post-processing.