In this study, boron doped and undoped poly (vinyl) alcohol/bismuth-gadolina acetate (PVA/Bi-Gd) nanofibers were prepared using electrospinning technique then calcinated at 800 degrees C for 2 h. The originality of this study is the addition of boron to metal acetates. The effects of boron doping were investigated in terms of solution properties, morphological changes and thermal characteristics. The characteristics of the fibers were investigated with FT-IR, XRD, SEM and BET. The addition of boron did not only increase the thermal stability of the fibers, but also their diameters, which yielded stronger fibers. XRD analyses showed that boron doping increased the peak intensities and indicated that the boron doping enhanced the crystallite size. Moreover, no shifts were noticed in diffraction angles for boron doped and undoped samples. Therefore, boron doping did not significantly alter the lattice spacing. The SEM micrograph of the fibers showed that the addition of boron resulted in the formation of cross-linked bright-surfaced fibers. The average fiber diameter for boron doped and undoped fiber mats were 204 and 123 nm, respectively. Also, grain diameters of boron doped and undoped nanocrystalline sintered powders were measured as 140 and 118 nm, respectively. The BET results showed that boron undoped and doped Bi2O3-La2O3 nanocrystalline powder ceramic structures sintered at 800 degrees C have surface areas of 59.72 and 39.80 m(2)/g, respectively.