多孔PZT95/5铁电陶瓷材料研究进展

基于铁电材料冲击波去极化效应的高功率脉冲电源在国防和高新技术领域具有重要应用。PZT95/5铁电陶瓷是目前铁电体高功率脉冲电源应用的理想材料。近年来, 多孔PZT95/5铁电陶瓷被发现具有更优异的综合性能而引起广泛关注。本文概述了多孔PZT95/5铁电陶瓷在微结构与性能调控、冲击波加载下的响应行为以及抗冲击损伤机制等方面的最新进展。研究发现, 具有合适气孔率和气孔分布的多孔PZT95/5铁电陶瓷具有优异的抗冲击损伤和耐电击穿性能; 多孔脆性材料中破碎介质的“滑移与转动”变形机制增强了材料的塑性变形, 从而提高了多孔材料的抗冲击损伤性能。最后, 简要介绍了BNT基无铅铁电陶瓷以及PIN-PMN铁电单晶在高功率脉冲电源方面应用的研究进展, 并对未来研究工作提出展望。     

Study on microstructure, piezoelectric and dielectric properties of 3-3 porous PZT composites

Porous lead zirconate titanate (PZT) composites are used for low frequency hydrophones due to their high hydrostatic figure of merit, and low sound velocity. Porous PZT composite materials manufactured using varied percentage of polymethyl methacrylate (PMMA) as a pore-forming agent was studied, to understand the effect of PMMA on microstructure and dielectric properties. Properties such as the density, porosity, transverse piezoelectric coefficient, dielectric constant, and dielectric loss factor were studied as a function of PMMA. Porous PZT composites (with 30% PMMA) show lower piezoelectric transverse coefficient (−78 pC/N) and dielectric constant (116) as compared to homogeneous PZT. At a frequency of 1 MHz, the dielectric constant decreases and dielectric loss increases with increase in PMMA. This paper describes the effect of polymethyl methacrylate (PMMA) as a pore-forming agent on dielectric properties and microstructure of porous PZT composites.     

致密PZT95/5铁电陶瓷低温相结构与电性能研究

采用固相法制备了致密PZT95/5铁电陶瓷, 研究了低温下致密PZT95/5铁电陶瓷相结构和电性能的变化规律。变温X射线衍射(XRD)研究表明, 低温(-60℃)下极化和未极化致密PZT95/5铁电陶瓷相结构保持不变。电性能研究表明随着温度从30℃下降至-60℃, 致密PZT95/5铁电陶瓷的相对介电常数从278显著下降至173, 而电阻率和剩余极化强度基本保持不变。结合冲击波载荷下动态放电模拟分析, 发现相对介电常数的降低将引起动态电场增大至常温下的1.5倍, 这可能是导致致密PZT95/5铁电陶瓷低温下击穿概率显著增大的关键因素。     

多孔PZT95/5铁电陶瓷的机械性能和铁电性能研究

采用添加造孔剂的方法制备多孔锆钛酸铅(PZT95/5)铁电陶瓷, 研究了孔结构包括孔隙率、孔径及孔形状对多孔PZT95/5陶瓷机械性能和电性能的影响及机理, 并揭示多孔PZT95/5陶瓷微观结构、机械性能和铁电性能的内在联系。研究表明: 孔隙率的增加降低了多孔PZT95/5陶瓷的声阻抗, 改善了陶瓷与封装材料的声阻抗匹配. 孔隙率增加, 多孔PZT95/5陶瓷的屈服应力和剩余极化强度降低, 矫顽场强增大。孔结构对多孔PZT95/5陶瓷屈服应力的影响可由应力集中理论解释; 多孔PZT95/5陶瓷剩余极化强度随孔结构的变化可用内应力结合空间电荷理论加以解释。     

包覆成孔剂法制备高性能多孔氮化硅陶瓷工艺

为了制备高强度且分布均匀的氮化硅陶瓷,采用包覆成孔剂法改进普通添加成孔剂的方法,常压烧结氮化硅多孔陶瓷,采用阿基米德法、三点弯曲法分别测试材料的孔隙率及抗弯强度,用扫描电镜和光学放大镜对氮化硅多孔陶瓷显微结构和表观结构进行研究.结果表明,添加包覆过的成孔剂强度比添加未包覆的成孔剂强度高,孔隙率为50%时,强度增加近一倍.强度的提高归因于特殊的微观结构,即气孔的均匀分布和孔与孔之间相间隔分布.     

铌镁酸铅-钛酸铅陶瓷介电与压电性能的研究

用二步合成法制备了（１－ｘ）Ｐｂ（Ｍｇ１／３Ｎｂ２／３）Ｏ３－ｘＰｂＴｉＯ３原料,并制成了纯钙钛矿结构压电陶瓷。研究三方－四主相界附近组份及工艺与性能的关系。材料以１２００℃附近保温１５０ｍｉｎ为佳。材料性能表明,有希望成为新型压电陶瓷。     

Enhanced ferroelectric properties of Pb(Zr0.80Ti0.20)O3/PbO thin films prepared by radio frequency magnetron sputtering

The Pb(Zr_0.80Ti_0.20)O₃ (PZT) thin films with and without a PbO buffer layer were deposited on the Pt(1 1 1)/Ti/SiO₂/Si(1 0 0) substrates by radio frequency (rf) magnetron sputtering method. The PbO buffer layer improves the microstructure and electrical properties of the PZT thin films. High phase purity and good microstructure of the PZT thin films with a PbO buffer layer were obtained. The effect of the PbO buffer layer on the ferroelectric properties of the PZT thin films was also investigated. The PZT thin films with a PbO buffer layer possess better ferroelectric properties with higher remnant polarization (P_r = 25.6 μC/cm²), and lower coercive field (E_c = 60.5 kV/cm) than that of the films without a PbO buffer layer (P_r = 9.4 μC/cm², E_c = 101.3 kV/cm). Enhanced ferroelectric properties of the PZT thin films with a PbO buffer layer is attributed to high phase purity and good microstructure.     

Damping property of epoxy-based composite embedded with sol–gel-derived Pb(Zr<Subscript>0.53</Subscript>Ti<Subscript>0.47</Subscript>)O<Subscript>3</Subscript> thin film

The Pb(Zr_0.53Ti_0.47)O₃ (PZT) thin films were prepared on Pt/Ti/SiO₂/Si substrate by sol–gel method. The effect of the annealing holding time on microstructure, ferroelectric and dielectric properties was investigated. The single-phase PZT films were obtained with different annealing holding time. PZT films annealed for 30–90 min had better dielectric and ferroelectric properties. The epoxy/PZT film/epoxy sandwich composites were prepared, and the annealing holding time of PZT films influenced the damping property of the composites. The epoxy-based composites embedded with PZT films annealed for 90 min had largest damping loss factor of 0.906.     

天线罩用多孔氮化硅陶瓷的制备

采用反应烧结工艺,通过添加成孔剂的方法,制备出具有球形宏观孔的低密度多孔氮化硅陶瓷,研究了球形宏观孔和烧结工艺对多孔氮化硅陶瓷性能的影响.实验结果表明,与未添加成孔剂的样品相比,成孔剂的添加有效降低了材料的气孔率,使材料的介电常数ε'和介电损耗tanδ下降.孔的加入能促进针状氮化硅的生成,降低单位体积中产生的热量,防止...     

Damping properties of epoxy-based composite embedded with sol–gel-derived Pb(Zr<Subscript>0.53</Subscript>Ti<Subscript>0.47</Subscript>)O<Subscript>3</Subscript> thin film annealed at different temperatures

Pb(Zr_0.53Ti_0.47)O₃ (PZT) thin films were prepared on Pt/Ti/SiO₂/Si substrate by sol–gel method. The effect of annealing temperature on microstructure, ferroelectric and dielectric properties of PZT films was investigated. When the films were annealed at 550–850 °C, the single-phase PZT films were obtained. PZT films annealed at 650–750 °C had better dielectric and ferroelectric properties. The sandwich composites with epoxy resin/PZT film with substrate/epoxy resin were prepared. The annealing temperature of PZT films influenced their damping properties, and the epoxy-based composites embedded with PZT film annealed at 700 °C had the largest damping loss factor of 0.923.     

0-3型(PZT,KTN)/P(VDF-TrFE)三相铁电复合材料的电学性能

以偏氟乙烯-三氟乙烯（P（VDF-TrFE））共聚物为基体,锆钛酸铅（PZT）铁电颗粒为功能相,钽铌酸钾（KTN）颗粒为增强相,制备了0-3型（PZT,KTN）/P（VDF-TrFE）三相铁电复合材料。利用SEM及EDAX技术,分析了复合材料的显微结构及PZT和KTN相的分布。测试了具有不同KTN 体积分数的复合材料的电性能。实验结果表明:PZT和KTN相的颗粒分布均匀,存在少量的团聚体;随KTN体积分数的增加,三相复合材料的极化漏电流I、介电常数ε_r和介电损耗tanδ增加,压电系数d₃₃降低,而热释电系数p₃先增加后降低,但其d₃₃和p₃均高于具有相同PZT体积分数的PZT/P（VDF-TrFE）两相复合材料。      

Electrophoretic deposition of lead zirconate titanate (PZT) powder from ethanol suspension prepared with phosphate ester

The formation of thick PZT films via electrophoretic deposition (EPD) was studied. The colloidal suspension of a nano-sized PZT powder dispersed in ethanol was prepared using a phosphate ester (PE) as a dispersant. The amount of PE addition on the stability of the PZT suspension has been investigated by measuring the pH and conductivity of the suspension, deposition weight and the relative density of the PZT green compacts. The effect of the applied voltage on the relative green density was also determined as a function of the wt% PE. The composition and microstructure of the sintered PZT ceramics were characterized by XRD and SEM. The electrical properties of the PZT ceramics were also investigated.     

锰掺杂对硬性PZT材料压电性能的影响

研究了锰掺杂对ＰＺＴ材料微结构及压电性能的影响,并用ＥＳＲ确定了锰在ＰＺＴ材料中的价态．结果表明,锰在ＰＺＴ材料中主要以 Ｍｎ^２＋和 Ｍｎ^３＋的方式共存．锰在ＰＺＴ陶瓷材料中的“溶解度”约为１．５ｍｏｌ％．锰含量＜０．５ｍｏｌ％时,Ｍｎ将以Ｍｎ^２＋和Ｍｎ^３＋的方式优先进入晶格 Ｐｂ位,使材料的压电性能提高,表现出施主杂质特性;锰浓度处于 ０．５～１．５ ｍｏｌ％时,部分Ｍｎ将以Ｍｎ^３＋或Ｍｎ^２＋的方式进入晶格中（Ｚｒ;Ｔｉ）位,而此浓度范围内锰掺杂的ＰＺＴ材料同时表现出“软性”和“硬性”材料的压电特性．锰含量＞１．５ｍｏｌ％时,过量的Ｍｎ将在晶界积聚,使压电活性降低．少量Ｆｅ的存在,可使Ｍｎ离子的溶解度降低,并起到抑制Ｍｎ^２＋和 Ｍｎ^３＋氧化的作用.     

Fabrication of Lead Zirconate Titanate Powder Using Ultrasonic Ball Milling Technique

In this research, the ultrasonic ball milling technique has been used to fabricate lead zirconate titanate （PZT） ceramics. PZT with the composition nearly the morphotropic phase boundary （MPB） ： Pb（Zr0.52 Ti0.48 ）03 was studied. The effect of milling time on phase formation of sample powder was examined by X-ray diffraction technique （XRD）. Moreover, the physical, dielectric, piezoelectric properties and microstructure of PZT ceramics were investigated. The present results reveal that the ultrasonic ball milling technique results the homogeneous and small size of PZT powder. Furthermore, there is a significantly change occurs in the size of the particles with the short time of milling process.     

(Bi0.5Na0.5)TiO3(BNT)基无铅压电陶瓷研究进展

(Bi0.5Na0.5)TiO3(BNT)基无铅压电陶瓷体系是目前研究最广泛的功能陶瓷材料之一.综述了BNT基无铅压电陶瓷的研究现状,讨论了相关体系的设计方法、铁电性、压电性以及BNT体系的制备方法.分析比较了BNT系压电陶瓷与Pb(Zr,Ti)O3(PZT)压电陶瓷的性能差异以及存在的问题,对BNT基无铅压电陶瓷进行了展望.     

Electron emission and phase transition of Zr-rich lead zirconate titanate ferroelectrics

This letter focuses on understanding the influences of antiferroelectric–ferroelectric (AFE–FE) phase transition on the ferroelectric electron emission process. The piezoelectric constant and electron emission current of un-prepoled PZT 96.5/3.5 ceramics as a function of emission times were studied. The hysteresis loops of PZT 96.5/3.5 ceramics before and after the electron emission process were presented. The results show that emission currents obtained from PZT 96.5/3.5 ferroelectrics in different phase states were similar. It was difficult to explain the experiment results using the fast AFE–FE phase transition model. Electron emission from PZT 96.5/3.5 ferroelectrics was independent of the AFE–FE phase transition.     

PZT95/5铁电陶瓷晶粒度对冲击波作用下击穿电压的影响

在气炮加载条件下,分别测试了两种晶粒度的PZT95/5铁电陶瓷样品在冲击波作用下的击穿电压,并采用Weibull分布分析了所获得数据.结果表明,PZT95/5铁电陶瓷在冲击波作用下的击穿电压分布可以用二参数Weibull分布模型描述,从击穿电压密度分布函数和失效率函数来看,晶粒度为2.5μm的PZT95/5样品的击穿电压分布优于晶粒度为7μm的PZT95/5样品击穿电压分布.     

轻质多孔陶瓷的制备及吸声性能研究

通过模压法成功制备轻质多孔陶瓷吸声材料, 采用JTZB吸声系数测试系统研究造孔剂粒径、含量以及样品厚度对多孔陶瓷材料吸声性能的影响。结果表明: 造孔剂含量为50vol%时, 大孔径多孔陶瓷吸声性能优于小孔径多孔陶瓷; 随着造孔剂含量的增加, 第一吸收峰从低频向高频移动, 峰值从0.41增加到0.82, 孔隙率过高和过低都不利于提高材料吸声性能; 样品厚度从10 mm增加到30 mm, 第一吸收峰逐渐向着低频方向移动; 造孔剂含量为60vol%, 样品厚度为20 mm时, 样品整体具有优异吸声性能, 并逐层在其背后加入空腔发现, 随着空腔层数的增加, 样品的第一吸收峰从高频向低频移动, 平均吸声系数逐渐增大。     

Conduction analysis of Li2O doped 0.2[Pb(Mg1/3Nb2/3)]–0.8[PbTiO3–PbZrO3] ceramics fabricated by columbite precursor method

We have fabricated 0.2Pb(Mg_1/3Nb_2/3)O₃–0.8Pb(Zr_0.475Ti_0.525)O₃ [PMN–PZT] ceramics doped with various amounts of Li₂O (0, 0.05, 0.1, 0.2, 0.3 wt.%) using the columbite precursor method. The effects of Li-doping on the conduction behavior of PMN–PZT ceramics are discussed in relation to the low frequency dielectric dispersion and frequency domain measurement. The Li-doped PMN–PZT ceramics sintered at 950 °C showed a sufficient densification with large dielectric constant and low dielectric loss. The incorporation of Li⁺ ion in PMN–PZT ceramics led to an appreciable reduction in electrical conductivity and further enhanced the ferroelectric and piezoelectric properties. The activation energies of PMN–PZT + xLi₂O (x = 0, 0.05, 0.1, 0.2, 0.3 wt.%) ceramics calculated from ac conductivity measurement using the Arrhenius relation were 1.05, 1.25, 1.27, 1.38 and 1.41 eV, respectively. The conduction behavior is examined in the low frequency and high temperature region and the results are discussed in detail through crystal defect mechanism.     

Sm掺杂增强PZT基弛豫型铁电陶瓷压电性能研究

锆钛酸铅(PZT)基压电陶瓷是一类应用非常广泛的功能材料, 可应用于水声换能器、压电马达、医疗超声换能器以及声表面波滤波器等。通过改性提高PZT基压电陶瓷的压电性能一直是该领域的研究热点。本工作采用传统固相反应法制备了准同型相界(Morphotropic Phase Boundary, MPB)组分的Sm-0.25PMN-0.75PZT压电陶瓷, 并对其微观结构以及宏观性能进行了系统研究。研究结果表明：引入Sm³⁺可以增强压电陶瓷的局域结构异质性, 提升介电响应从而提高压电性能。当Sm³⁺引入过多时, 铁电极化的长程连续性被大面积打断, 压电性能下降。本实验中得到的最优组分压电陶瓷性能为：高压电系数d₃₃~824 pC/N, 高压电电压常数g₃₃~27.1×10^-3 m²/C和相对较高居里温度T_C~178 ℃, 电致应变在室温至150 ℃范围内低于5%, 有较好的温度稳定性, 是极具应用前景的高性能压电材料。