类单晶PZT纳米纤维的静电纺丝制备探索
王 娟，贺海晏，高 倩，李 铭，李 翔*，韩高荣*
（浙江大学材料科学与工程学系 无机非金属材料研究所，浙江 310027）
摘 要：以硝酸锆（Zr(NO3)4•5H2O），乙酸铅（Pb(CH3COO)2•3H2O），钛酸四丁酯（Ti(OC4H9)4）和聚乙烯吡咯烷酮（PVP）为原料，采用sol-gel和静电纺丝法，结合烧结工艺首次制备了在准同型相界附近的类单晶PZT纳米纤维。利用热重分析、X射线衍射仪、扫描电镜和透射电镜等表征方法，对类单晶PZT纤维的热分解过程、晶体结构、微观相貌和形成机理等进行了分析和解释。研究结果表明：经过400°C预退火0.5 h以及750°C烧结2 h后，可形成具有类单晶结构的PZT纳米纤维，纤维直径约在80 ~100 nm左右，晶体结构为典型的钙钛矿相。形成这种类单晶结构的主要机理是在预退火期，有机物充分分解形成无规则非晶网络，随着烧结温度的升高，取向基本一致的小晶粒经历了形核、长大、吞噬，最终形成类单晶纳米纤维。在准同型相界附近的类单晶PZT纳米纤维在纳米压电器件和微机电系统领域具有广泛的应用前景。
关键词：类单晶；锆钛酸铅；静电纺丝
中图分类号：TB381；TB383；TG115.21+5.3 文献标识码：A
Exploration of single-crystal like electrospun Pb(Zr0.52Ti0.48)O3 nanofibers synthesis via electrospinning
WANG Juan,HE Hai-yan, GAOQian, LI Ming, LIXiang*, HAN Gao-rong*
(Inorganic Nonmetallic Materials Institute, Department of Materials Science and Engineering, Zhejiang University, Hangzhou Zhejiang 310027,China)
Abstract:Single-crystal-like lead zirconate titanate (PbZr0.52Ti0.48O3, PZT) ceramic fibers were successfully prepared by sol-gel based electrospinning and subsequent calcination process. The thermo-decomposition process, fiber morphology, crystal structure and formation mechanism of the single-crystal-like PZT nanofibers were characterized using the thermogravimetry/differential scanning caborimetry (TG/DSC), X-ray diffraction (XRD) and transmission electron microscopy (TEM). The fiber was smooth and uniform with a diameter of ~80 to ~100 nm. The crystal structure of the nanofibers pyrolyzed at 400°C for 0.5 h and calcined at 750°C for 2 h was proved to be single-crystal-like tetragonal perovskite phase. The formation mechanism was proposed as follows: For the pyrolysis process, the polymer was decomposed completely; When the calcination temperature increased, the new-formed nanocrystallites oriented growed at the nuclei sites and aggregated into large single crystals of preferred orientation that retain the morphology of the original shape. Such single-crystal-like PZT nanofibers with a near MPB composition have therefore been a milestone for piezoelectric nanodevices with significantly enhanced performance.
Keywords:single-crystal-like；PZT nanofibers；electrospinning
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