This study is related to the preparation of boron doped Nickel/Zinc metal fibers prepared by the use of electrospinning technique. The originality of this study is the addition of boron to metal acetates. The addition of boron did not only increase the thermal stability of the fibers, but also increased their diameters, which gave stronger fibers. The FT-IR spectra of the fibers were in good accordance with literature. The differential scanning calorimetry (DSC) results indicate that the glass transition (Tg) and melting temperatures (Tm) showed great change with the addition of boron and boron doped fibers were observed to degrade at higher temperatures. The SEM appearance of the fibers showed that the addition of boron resulted in the formation of cross linked bright surfaced fibers.