Synthesis of La and Nb doped PZT powder by the gel-combustion method

Lanthanum and niobium doped PZT with composition (Pb0.93La0.07)[(Zr0.60Ti0.40)]0.9825Nb0.0175O3 (PZTLN) was prepared by the gel-combustion method. A precursor sol was obtained from lead nitrate, zirconyl nitrate, lanthanum oxide, peroxo-citrato-niobium and a peroxo-citrate complex of titanium isopropoxide as starting precursors. Various molar ratios of citrate/nitrate (CA/NO3(-) = 1.3, 0.36 and 0.09) were used to prepare very fine powders of PZTLN. The gels resulting from these sols were transformed into powders by an auto-combustion process at ≤400 °C. The powders consisted of rhombohedral PZT (PbZr0.60Ti0.40O3), pyrochlore (Pb2Ti2O6) and lead carbonate (Pb2O·CO3) phases. The pure rhombohedral phase is found in PZTLN pellets sintered at 1100 °C for all citrate/nitrate ratios. Titanium and niobium precursors were modified with peroxo radicals. During the gel-combustion reaction, the temperature of the gel increases, leading to lead evaporation. The loss of lead as well as the particle size increases as the CA/NO3(-) ratio decreases. The smallest grained powder (about 50 nm) was obtained with the ratio CA/NO3(-) equal to 0.09.