Ferroelectric/ferromagnetic multiphase powdered composites, consisting of PbTiO3 as ferroelectric phase and NiFe2O4 (PbFe12O19) as ferromagnetic phase, were successfully prepared in situ by sol-gel process. The phase structure, morphology and magnetism properties were observed. Biphase powdered ME composite consisting of PbTiO3 and NiFe2O4 is obtained at 700oC. Triphase composite consisting of PbTiO3, NiFe2O4 and PbFe12O19 is obtained above 750oC. With increasing heat-treatment temperature, the particles combine more tightly and the particle size decreases. The saturation magnetization (σs) and the initial permeability (μi) increase with the increase of NiFe2O4 content. The coercive force (Hc) increases with the increase of PbFe12O19 content.