Barium titanate, BaTiO₃ [BT] and Barium calcium titanate-zirconate BaCa(Ti Zr)O₃ [BCTZ] powders were prepared utilizing sol gel polymeric method using urea formaldehyde resin, as a template. The obtained gel dried at 80°C/48h, then calcined at different temperature 800, 1000 and 1100°C/3h. FT-IR analysis, thermal analysis in terms of DTA-TG were carried to the polymer gel, and gel hosting cations at 80°C. Phase composition using X-ray diffraction (XRD) was investigated to the calcined powder at the previous temperatures, Microstructure using scanning electron microscopy (SEM) was studied at 1100°C/3h. It was found that the pure perovskite of (Tetragonal-orthorhombic-monoclinic) barium titanate [BT] and (Tetragonal-orthorhombic-monoclinic) [BCTZ] powder was obtained at a calcination condition of 1100 °C for 3h.The average crystal size 24.14 nm for BT powder  while BCTZ powder recorded 22.83 nm. Uniform grain microstructure powders contain nearly spherical pores was obtained