In Ni -doped YBCO systems, Ni ions have been generally thought to enter Cu (2) sites; in fact, the relevant arguments never ceased in the past decade, because various experimental results have not achieved a definite and consistent conclusion. The present paper systemically investigates YBa 2 Cu 3-x Ni x O 7-δ(x = 0~0.4) cuprates with X-ray diffraction, positron annihilation technique, and simulated calculations. The results show that Ni ions enter Cu (2) sites at the low-doped concentration, as the concentration increases, a certain proportion of Ni ions begin to enter the Cu (1) sites until the appearance of the impurity phase.