In this paper, we report a strategy for hybrid multiferroicity at nanoscale. Multiferroic NiFe2O4-Pb(Zr0.52Ti0.48)O-3 composite nanofibers are synthesized by a sol-gel process and electrospinning, with fiber diameters ranging from 100 to 400 nm. Energy dispersive spectroscopy and transmission electron microscopy indicate that nanocrystalline Pb(Zr0.52Ti0.48)O-3 and NiFe2O4 grains are randomly distributed in the composite nanofibers, with grain size around 30 nm. The spinel structure of NiFe2O4 and the perovskite structure of Pb(Zr0.52Ti0.48O3) are verified by x-ray diffraction, and multiferroicity of the nanofibers is confirmed by piezoresponse force microscopy and magnetic hysteresis. The structures and properties of the composite nanofibers are also compared with single-phase Pb(Zr0.52Ti0.48)O-3 and NiFe2O4 nanofibers. These composite nanofibers could lead to unconventional multiferroic structures and devices. (c) 2008 American Institute of Physics.