Preventing the formation of the pyrochlore phase in the synthesis of PZN-PT powders requires controlling calcination parameters such as temperature, soaking time and atmosphere. These parameters were examined extensively to determine the time and temperature at which the perovskite phase is the majority phase, as well as the atmosphere that facilitates the formation of this phase. A maximum of 74% of perovskite phase was obtained under the following conditions: 1000 °C, 4 h in nitrogen atmosphere. In this work, we studied the influence of these parameters, which were optimized, on the formation the perovskite phase in PZN-10PT powders synthesized by the conventional solid state method.