In this study, hydroxyapatite/polyvinyl alcohol (HAp-PVA) biocomposites were prepared using a spray drying method. HAp-PVA solutions fed to spray dryer were prepared by two different routes, namely, physical and in situ biomimetric methods. In the former method, HAp was synthesized without the presence of polymer and then HAp particles were incorporated into a PVA solution. In the second one, hydroxyapatite was in situ synthesized in the presence of PVA. Experiments were also run to investigate the effect of the molecular weight of PVA on the structure of spray-dried biocomposites. Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy and particle size analyses were performed to characterize the produced HAp-PVA composites.