This work deals with an experimental investigation of the microstructure/morphology of spin-casted composite thin films of poly(3-hexylthiophene) (P3HT) and silicon nanocrystals (Si-NCs), in the weight proportion 1:1, which develop under different deposition conditions. The experimental parameters considered were the following: i) solvent quality; ii) spinning rate; iii) spinning time and iv) solution concentration. The developed morphologies were characterized by means of optical microscopy and X-ray diffraction (XRD) measurements. The present work aims at a) establishing the relationship between processing conditions and resultant morphology and b) defining the most relevant processing parameters that govern and are of significance for the induced morphology.