Electrospinning process is the useful and unique method to produce nanofibers from metal precursor and polymer solution by controlled viscosity. In this study, the NiZn ferrite nanofibers were prepared by electrospinning with a aqueous metal salts/polymer solution that contained polyvinyl pyrrolidone and Fe (III) chloride, Ni (II) acetate tetrahydrate and zinc acetate dihydrate in N,N-dimethylformamide. The applied electric field and spurting rate for spinning conditions were 10 kV, 2 ml/h, respectively. The obtained fibers were treated at $250^{circ}C$ for 1 h to remove the polymer. Finally, the NiZn ferrite fibers were calcined at $600^{circ}C$ for 3 h and annealed at $900{sim}1200^{circ}C$ in air. By tuning the viscosity of batch solution before electrospinning, we were able to control the microstructure of NiZn ferrite fiber in the range of $150{sim}500;nm$ at 770 cP. The primary particle size in $600^{circ}C$ calcined ferrite fiber was about 10 nm. The properties of those NiZn ferrite fibers were determined from X-ray diffraction analysis, electron microscopy, energy dispersive spectroscopy, Fourier transform infrared spectroscopy, thermal analysis, and magnetic measurement.