Preparation and Characterization of Pb(Zr 0.52 Ti 0.48 )O 3 Powders and Thin Films by a Sol-gel Route
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ngxi Zhang School of Science, Harbin Institute of Technology, P.O. Box 408, Harbin 150001, People’s Republic of China
Zhong Wang and Liancheng Zhao School of Materials Science and Engineering, Harbin Institute of Technology, P.O. Box 433, Harbin 150001, People’s Republic of China (Received 16 July 1998; accepted 8 March 2000)
Lead zirconate titanate [Pb(ZrxTi1−x)O3 (PZT)] powders and ferroelectric thin films with a composition near the morphotropic phase boundary [Pb(Zr0.52Ti0.48)O3] were prepared by a modified sol-gel process using zirconium oxynitrate-2-hydrate as the zirconium source and ethylene glycol as solvent. The precursor solution was prepared from lead acetate-3-hydrate, tetrabutyl titanate, and zirconium oxynitrate-2-hydrate. Perovskite PZT powders were obtained after sintering at 450 °C for 2 h. Films rapid-thermally annealed at 650 °C for 1 min formed well-crystallized perovskite. Microstructures of these films indicated the presence of nano-sized grains (∼50 nm). The remnant polarization was 28.5 C/cm2, and the coercive field was 39.8 kV/cm. Ferroelectric polarization fatigue test of In/PZT/Pt/Ti/SiO2/Si showed a high fatigue resistance up to 3 × 1010 cycles before Pr decreased by 50%.
I. INTRODUCTION
The sol-gel process has attracted considerable interest in the fabrication of multicomponent oxide thin films,1,2 bulk powders,3 and ceramics,4 because it offers high purity, chemical homogeneity, and controlled particle sizes of ceramics. Besides lowering processing temperatures, the main advantages of this process is in achieving chemical homogeneity of the desired product due to intimacy of mixing of the constituents at the molecular level.5 Recently, there has been an unprecedented interest in the processing of polycrystalline ferroelectric thin films, especially of solid solution in the multiaxial perovskite lead zirconate titanate system, due to the growing demand for compatibility with integrated circuit (IC) planar technology. Potential applications in thin film form include optical shutters, displays and modulators, piezoelectric microtransducers and microsensors, ferroelectric gate field-effect transistor (FET), non-volatile memories, high dielectric constant dielectric layers in ULSI DRAM, decoupling capacitors, and infrared (IR) detection and imaging components.6 Lead zirconate titanate (PZT) thin films with morphotropic phase bounda)
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J. Mater. Res., Vol. 15, No. 6, Jun 2000 Downloaded: 12 Mar 2015
ary composition ([Zr]/[Ti] ⳱ 52/48) have received much attention because they have low coercive fields and high remnant polarization.7 Sol-gel processing of perovskite ABO3-type ceramics generally involves the following steps: (i) preparation of a clear solution containing the A and B constituents in the required stoichiometry; (ii) hydrolysis of the solution leading to the formation of polymeric -(A–B–O)-network (gel) through condensation reactions; and (iii) conversion of the gel to th
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