A series of Pb 1−x Ni x TiO 3 (x = 0, 0.1, 0.2, 0.3, 0.4 and 0.5) were prepared by the general ceramic and co-precipitation method. The grain size decreased with increasing Ni contents. The piezoelectric modulus d 33 increased with increasing Ni contents. It was observed also the d 33 of the nanocomposite Pb 1−x Ni x TiO 3 prepared by co-precipitation method is higher than those of the prepared by general ceramic method. The coupling factor k p increased by the more doping of Ni. The ultrasonic wave velocity decreased also with increasing Ni contents. The polarized nano-sample of composition Pb 0.5 Ni 0.5 TiO 3 is suitable for improving application of useful piezoelectric technology.