| In this work, tetragonal crystal lead zirconate titanate (PZT) powders with the particle size ranged from 0.1～1.5μm were prepared by solvothermal process which is developed from hydrothermal method at a low temperature. Pb(NO3)2, ZrOCl2—8H2O and TiCl4 were used as raw materials, KOH as mineralizer and a mixture of ethanol and water with different volume ratio as reactive solvent. The influence of reactive temperature, time, basicity, molar ratio of Pb/(Zr +Ti), total reactants concentration, ultrosound and volume ratio of ethanol and water on the phase, morphology and partilce size of PZT powders were studied.The results showed that PZT average particle size decreased from 1.25 to 0.1μm with the ratio of ethanol to water increasing from 1:4 to 4:1. The lower temperature and basicity were needed to prepare PZT powders when the mixed solvents of ethanol and water was uesd as reactive medium compared with water solvent. Higher temperature was favourable for the preparation of smaller size PZT powders. The particle size of powders decreased from 1.5μm to 0.8μm with the increase of the temperature from 140℃to 200℃. When the alkali concentration increased from 1 to 4mol/L, the particle size decreased from 1.2μm to 0.1μm. With Pb/(Ti+Zr) increased from 1.0 to 1.9, the particle size increased from 10 nm to 1.3μm and it is essential to make sure Pb/(Ti+Zr)=1.5 to obtain well-crystalline PZT powders, As reactants concentration increased the particle size showed slight descent. Soaking time had a restrain effect on the particle size.The particle size of PZT powders obtained from reactive precursor which was dispersed by ultrasound was far smaller than that came from the precursor dispersed by mechanical method. Tetragonal PZT powders with particle size about 0.8μm can be obtained when suitbale condition,were solventhermal temperature of 160℃, alkali concentration of 2mol/L, volume ratio of ethanol to water of 2:1, total reactants concentration of 1mol/L, time of 0.5h and Pb/(Ti+Zr) of 1.5. |
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