In this study, polyvinyl alcohol (PVA) and boric acid (BA) were mixed in an aqueous medium by heating in order to prepare a PVA/BA hybrid material. The viscosity and pH values of the PVA/BA hybrid material mixed in various proportions were determined. Then the hybrid polymer was electrospun to give dimensions to fibers. The FT-IR spectra of these fibers revealed that BA chemically reacted with PVA and formed B-O-C bonds. The fibers were first calcified at 500 degrees C and then the calcified products were pelleted and exposed to the sintering process at 1300 degrees C. The XRD peaks of the sintered product were seen at 2 theta = 34.7 and 37.7 degrees verified the formation of boron carbide. The study proved that it was possible to use sub-micron fibers for the production of sub-micron boron carbide material.