One-dimensional and quasi-one-dimensional nanostructure materials are promising building blocks for electromagnetic devices and nanosystems. In this work, the composite Ni0.5Zn0.5Fe2O4(NZFO)/Pb(Zr0.52Ti0.48)O-3(PZT) nanofibers with average diameters about 65 nm are prepared by electrospinning from poly(vinyl pyrrolidone) (PVP) and metal salts. The precursor composite NZFO/PZT/PVP nanofibers and the subsequent calcined NZFO/PZT nanofibers are investigated by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM). The magnetic properties for nanofibers are measured by vibrating sample magnetometer(VSM). The NZFO/PZT nanofibers obtained at calcination temperature of 900 degrees C for 2 h consist of the ferromagnetic spinel NZFO and ferroelectric perovskite PZT phases, which are constructed from about 37 nm NZFO and 17 nm PZT grains. The saturation magnetization of these NZFO/PZT nanofibers increases with increasing calcination temperature and contents of NZFO in the composite.