Spinel-perovskite multiferroics of NiFe2O4/BiFeO3 nanoparticles were prepared by modified Pechini method. The structure and morphology of the composites were examined by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results showed that the composites consisted of spinel NiFe2O4 and perovskite BiFeO3 after annealed at 700°C for 2h, and the particle size ranges from 40 to 100nm. VSM and ME results indicated that the nanocomposites exhibited both tuning magnetic properties and a ME effect. The ME effect of the nanocomposites strongly depended on the magnetic bias and magnetic field frequency.