Perovskite phase formation and ferroelectric properties of the lead nickel niobate–lead zinc niobate–lead zirconate titanate ternary system Naratip Vittayakorn, Gobwute Rujijanagul, and Tawee Tunkasiri Department of Physics, Faculty of Science, Chiang Mai University, Chiang Mai 50200 Thailand Xiaoli Tan and David P. Cann Materials Science and Engineering Department, Iowa State University, Ames, Iowa 50011 (Received 23 June 2003; accepted 24 September 2003) The ternary system of lead nickel niobate Pb(Ni 1/3 Nb 2/3 )O 3 (PNN), lead zinc niobate Pb(Zn 1/3 Nb 2/3 )O 3 (PZN), and lead zirconate titanate Pb(Zr 1/2 Ti 1/2 )O 3 (PZT) was investigated to determine the influence of different solid state processing conditions on dielectric and ferroelectric properties. The ceramic materials were characterized using x-ray diffraction, dielectric measurements, and hysteresis measurements. To stabilize the perovskite phase, the columbite route was utilized with a double crucible technique and excess PbO. The phase-pure perovskite phase of PNN–PZN–PZT ceramics was obtained over a wide compositional range. It was observed that for the ternary system 0.5PNN–(0.5 - x)PZN–xPZT, the change in the transition temperature (T m ) is approximately linear with respect to the PZT content in the range x 0 to 0.5. With an increase in x, T m shifts up to high temperatures. Examination of the remanent polarization (P r ) revealed a significant increase with increasing x. In addition, the relative permittivity ( r ) increased as a function of x. The highest permittivities ( r 22,000) and the highest remanent polarization (P r 25 C/cm 2 ) were recorded for the binary composition 0.5Pb(Ni 1/3 Nb 2/3 )O 3 –0.5Pb(Zr 1/2 Ti 1/2 )O 3 . I. INTRODUCTION Lead-based complex perovskites, such as Pb(Zn 1/3 Nb 2/3 )O 3 (PZN) and Pb(Ni 1/3 Nb 2/3 )O 3 (PNN), having the general formula Pb(B'B)O 3 have received significant attention since the 1970s because of their peculiar dielectric and piezoelectric behavior. These materials have been ap- plied in many areas such as electrostrictive actuators, transducers, and multilayer ceramic capacitors. 1–6 Lead zinc niobate, PZN, was first synthesized in the 1960s. 7 Its permittivity versus temperature curve dis- played a broad peak around 140 °C (T m ) with a strong frequency dependence. Extremely high relative permit- tivities have been measured in the vicinity of the peak with a r 60,000 reported for single crystals. 4,8–11 Nanometer-level chemical heterogeneity in the form of short range order of Zn 2+ and Nb 5+ at B-sites was pro- posed to account for the observed diffuse phase transi- tion. 12,13 The crystal structure of PZN is rhombohedral (3m) at room temperature and transforms to cubic (Pm3m) at high temperatures. Unfortunately, phase-pure perovskite PZN polycrys- talline ceramics have not been synthesized by conven- tional solid-reaction methods because of a steric and an electrostatic interaction between high polarization of the Pb 2+ cation and the Zn 2+ cation, which favors the for- mation of the pyrochlore phase instead of the perovskite phase. 14 Moreover, the low tolerance factor and small electronegativity difference 2 makes the perovskite phase unstable, requiring the addition of normal ferroelectric compounds such as BaTiO 3 15 and PbTiO 3 16 to stabilize the perovskite phase. Recently, Fan et al. 17,18 mixed Pb(Zr 0.47 Ti 0.53 )O 3 with PZN by a conventional solid- state reaction method and successfully stabilized perov- skite PZN. A morphotropic phase boundary (MPB) between the PZN-rich rhombohedral phase and the PZT-rich tetragonal phase was reported at PZN:PZT47/53 1:1. At this composition, a high electromechanical coupling factor of k p 0.67 was measured. Lead nickel niobate (PNN) exhibits a diffuse phase transition around -120 °C with a much lower peak per- mittivity of about 4000. 19 The crystal structure of PNN at room temperature is cubic (Pm3m) with a lattice param- eter of 4.03 Å. 19 Phase-pure perovskite PNN can be prepared via the columbite method. 2,20 Luff et al. 21 investigated solid solutions in the PNN–PbTiO 3 –PbZrO 3 system and identified the composition of 0.5PNN– 0.35PT–0.15PZ with optimal piezoelectric properties. Detailed reaction kinetics during solid state processing of J. Mater. Res., Vol. 18, No. 12, Dec 2003 © 2003 Materials Research Society 2882 ÅÔ¢ÊÔ·¸ÔìÁËÒÇÔ·ÂÒÅÑÂàªÕ§ãËÁè Copyright by Chiang Mai University All rights reserved ÅÔ¢ÊÔ·¸ÔìÁËÒÇÔ·ÂÒÅÑÂàªÕ§ãËÁè Copyright by Chiang Mai University All rights reserved