PZT铁电薄膜纳米尺度铁电畴的场致位移特性

利用扫描力显微术的压电响应模式，并基于逆压电效应原理，研究了梯度组成的PZT铁电薄膜纳米尺度铁电畴的场致位移特性.获得了源于纳米尺度铁电畴的压电效应和电致伸缩效应贡献的场致位移回滞线，以及源于线性压电效应和电畴反转效应综合贡献的纳米尺度压电位移 场强蝶形曲线，证实了Caspari Merz理论在纳米尺度上的有效性.发现了梯度铁电薄膜存在纳米尺度印刻现象，认为该现象的内因源于薄膜中的内偏场. 关键词： PZT铁电薄膜 场致位移 纳米尺度 扫描力显微术     

PT/PZT/PT铁电薄膜的铁电畴和畴壁

用sol-gel法制备出了具有良好铁电性、纯钙钛矿结构的PbTiO₃/Pb(Zr_0.3Ti_0.7)O₃/PbTiO₃(PT/PZT/PT)新型夹心结构铁电薄膜.用扫描力显微镜(SFM)的压电响应模式获得了薄膜铁电畴的垂直于膜平面方向(OPP)、膜平面内(IPP)及OPP的相位和幅度图像，结合理论分析指出薄膜的电畴主要由c畴和偏离垂直于膜平面方向上的c畴构成，薄膜取向的复杂性导致了复杂的畴结构.对于［111］取向的薄膜，当偏离垂直于膜平面方向上的c畴在垂直膜平面方向和面内方向都相反时构成180°的畴壁，在垂直膜平面方向上相同、面内方向相反或由垂直膜平面方向上相反、面内方向相同时构成90°畴壁. 关键词： 铁电薄膜 PT/PZT/PT 电畴和畴壁 扫描力显微镜(SFM)     

锆钛酸铅薄膜的铁电疲劳微观机理及其耐疲劳性增强

铁电随机存储器(ferroelectric random access memory,FeRAM)因其卓越的数据存储性能与非易失性存储特性等优势而备受关注,但其自身固有的铁电疲劳失效问题制约了 FeRAM进一步的发展和商业化应用.FeRAM的疲劳失效与铁电薄膜的畴壁运动密切相关,但其内在疲劳机理仍有待深入研究.本文采用基于密度泛函理论(density functional theory,DFT)的第一性原理计算方法,研究了锆钛酸铅(Pb(Zr_(0.52)Ti_(0.48))O_3,PZT)的疲劳失效机理并提出了增强其耐疲劳性能的方法.计算结果表明:PZT中氧空位与180°畴壁运动的耦合是其铁电疲劳的内在原因,PZT铁电薄膜中越靠近畴壁的地方越容易形成氧空位,畴壁处大量氧空位对畴壁运动的"钉扎"作用使畴壁迁移困难,抑制了其极化反转最终导致了铁电疲劳;Ba(Mg_(1/)3Nb_(2/3))O_3 (BMN)缓冲层的存在可吸收PZT中的氧空位,降低畴壁处的氧空位浓度,提升其耐疲劳性能.实验结果表明,经过10~(10)次极化反转后,PZT铁电薄膜的剩余极化值降低了 51%,而PZT/BMN薄膜的剩余极化值仅降低了 18%;经过10~(12)次极化反转后,PZT/BMN薄膜的剩余极化值仍保持有82%并持续稳定.以上结果表明,BMN缓冲层引入确实能提高PZT铁电薄膜的耐疲劳性,有望满足FeRAM商业化应用的需求.     

极化状态与方向对单轴压缩下Pb(Zr_(0.95)Ti_(0.05))O_3铁电陶瓷畴变与相变行为的影响

利用数字图像相关性分析方法发展了全场应变光学测量技术,并原位实时测量了准静态单轴压缩下铁电PZT95/5陶瓷试件的轴向应变和横向应变.基于轴向应变、横向应变随着轴向应力的变化关系,讨论了极化状态和极化方向对PZT95/5铁电陶瓷的畴变与相变行为的影响.实验结果显示:单轴压缩下,未极化和Z轴极化PZT95/5铁电陶瓷都会发生畴变,而Y轴极化PZT95/5铁电陶瓷则不发生畴变;畴变促使Z轴极化PZT95/5铁电陶瓷的轴向应变和横向应变同时快速地增长,而对未极化PZT95/5铁电陶瓷的应变增长的影响非常微弱,这种差异性归因于电畴极轴不同的取向分布特征;通过应变分解分析,验证了畴变与相变过程是解耦的,并界定了畴变应变和相变应变的影响范围;与Z轴极化PZT95/5铁电陶瓷相比,未极化PZT95/5铁电陶瓷的相变开始临界应力和相变结束应力减小,而Y轴极化PZT95/5铁电陶瓷则明显增大,由此推论畴变对相变有一定促进作用.基于放电特性的实测结果,还讨论了极化方向对极化PZT95/5铁电陶瓷去极化机理的影响.实验结果显示:Z轴极化PZT95/5铁电陶瓷去极化机理是畴变和相变的共同作用,其中畴变占主导地位,而Y轴极化PZT95/5铁电陶瓷的去极化机理仅是相变.     

不同晶化工艺对非晶PZT纳米薄膜形核取向生长机理的影响

射频磁控溅射法室温下在Pt/Ti/SiO2/Si上制备非晶Pb(Zr048Ti052)O3薄膜，非晶PZT薄膜分别经常规炉退火(CFA)处理和快速热退火(RTA)处理晶化为（100），（111）不同择优取向的多晶薄膜. 采用x射线衍射测定了薄膜相组分、择优取向度；用原子力显微镜和压电响应力显微镜观察了薄膜表面形貌，以及对应区域由自发极化形成的铁电畴像，观察了不同取向薄膜的电畴分布特征. 结果表明，RTA晶化过程钙钛矿结构PZT结晶主要以PZT/Pt界面处的PtPb化合物为成核点异质形核并类似外延的结晶生长，沿界面结晶速率远大于垂直膜面结晶速率，而CFA晶化样品成核发生在膜内杂质缺陷处，以同质成核为主. 不同的成核机理导致了不同晶面择优取向生长. 关键词： PZT薄膜 结晶 形核 力显微技术     

微结构对Eu掺杂Bi4Ti3O12铁电薄膜铁电性能的影响

采用金属有机物分解法在Pt/Ti/Si(111)基底上制备了退火温度分别为600℃,650℃,700℃的Bi_3.15Eu_0.85Ti₃O₁₂(BET)铁电薄膜,并对其结构及铁电性能进行了测试,再使用扫描探针显微镜对BET薄膜的电畴翻转进行了实时观测.BET薄膜c畴发生180°畴变的最小电压为+6V,而r畴由于其高四方性,即使极化电压增至+12V也不会发生翻转.薄膜的铁电性主要源于c畴的极化,随着退火温度的升高,c畴的区域面积增加,BET薄膜的剩余极化强度随之增大.退火温度为700℃的BET薄膜剩余极化强度达到84μC/cm². 关键词： 铁电薄膜 电畴翻转 扫描探针显微镜     

多孔未极化Pb(Zr0.95Ti0.05)O3铁电陶瓷单轴压缩力学响应与相变

通过添加造孔剂的方法制备了四种不同孔隙率未极化PZT95/5铁电陶瓷. 采用非接触式的数字散斑相关性分析(digital image correltation, DIC)全场应变光学测量技术, 对多孔未极化PZT95/5 铁电陶瓷开展了单轴压缩实验研究, 讨论了孔隙率对未极化PZT95/5铁电陶瓷的力学响应与畴变、相变行为的影响. 多孔未极化PZT95/5铁电陶瓷的单轴压缩应力-应变关系呈现出类似于泡沫或蜂窝材料的三阶段变形特征, 其变形机理主要归因于畴变和相变的共同作用, 与微孔洞塌缩过程无关. 多孔未极化PZT95/5铁电陶瓷的弹性模量、压缩强度都随着孔隙率的增加而明显降低, 而孔隙率对断裂应变的影响较小. 预制的微孔洞没有改善未极化PZT95/5铁电陶瓷材料的韧性, 这是因为单轴压缩下未极化PZT95/5铁电陶瓷的断裂机理是轴向劈裂破坏, 微孔洞对劈裂裂纹传播没有起到阻碍和分叉作用. 准静态单轴压缩下多孔未极化PZT95/5铁电陶瓷畴变和相变开始的临界应力都随着孔隙率的增大而呈线性衰减, 但相变开始的临界体积应变却不依赖孔隙率.     

(111)取向(Pb,La)TiO3铁电薄膜中90°纳米带状畴与热释电性能的研究

采用射频磁控溅射技术在Pt/Ti/SiO₂/Si(100)衬底上生长了掺镧钛酸铅(PLT)铁电薄膜.用X射线衍射技术(XRD)研究了PLT薄膜结晶性能，结果表明PLT薄膜为 (111)择优取向钙钛矿相织构.使用原子力显微镜(AFM)和压电响应力显微镜(PFM) 分别观察了PLT薄膜的表面形貌和对应区域的电畴结构.PFM观察显示PLT薄膜中存在90°纳米带状畴，电畴的极化为首尾相接的低能量的排列方式，带状畴的宽度为20—60nm.研究了PLT10铁电薄膜的制备条件与性能之间的关系.发现在优化条件下制备的PLT10铁电薄膜的介电常数ε_r为365、介电损耗tgδ为0.02，热释电系数γ为2.18×10^-8C·(cm²·K)^-1，可以满足制备非制冷红外探测器的需要. 关键词： PLT薄膜 电畴 PFM 极化     

晶粒尺寸及衬底应力对铁电薄膜特性的影响

考虑衬底应力、畴壁运动和畴结构变化, 建立了修正的Landau-Devonshire热力学模型, 计算了生长在不同衬底上的含有纳米晶粒的PbZr_0.4Ti_0.6O₃(PZT)薄膜的电滞回线, 研究了矫顽场、剩余极化强度和相对介电常数对晶粒尺寸以及薄膜厚度的依赖关系. 结果表明, 矫顽场和相对介电常数对晶粒尺寸的依赖关系呈类抛物线状;衬底压应力使矫顽场和剩余极化强度增大, 使相对介电常数减小;随着厚度增加, 矫顽场先缓慢增加, 到200 nm 关键词： 铁电体 晶粒尺寸 衬底应力 薄膜厚度     

用改进的sol-gel法制备锆钛酸铅薄膜及其物相转化的研究

利用改进的solgel法,在Pt/Ti/SiO2/Si衬底上制备了PbZr0.5Ti0.5O3(PZT50/50)薄膜.采用了一种新的方式,从同一前驱体溶液得到了厚度各异的单一退火层.研究了薄膜的结构和性质随单层退火厚度的改变而发生的变化,发现随着单一退火层厚度的降低,薄膜(111)取向的程度增大,同时薄膜的剩余极化和介电常量也逐渐增高.当单一退火层厚度降低到约为40nm时,可得到高度(111)择优取向的PZT薄膜.从薄膜成核机理的基础上讨论了薄膜结构变化的内在因素,认为随单一退火层厚度的增加薄膜由单一的 关键词：     

Nanoscale domain switching mechanism in Pb(Zr,Ti)O<Subscript>3</Subscript> thin film

Pb(Zr,Ti)O₃ (PZT) ferroelectric thin film was prepared by the sol-gel technique and crystallized with a (111) preferred orientation. The domain structure and polarization reversal behavior were investigated by using scanning force microscopy (SFM) piezoresponse mode at the nanometer scale. A step structure of approximately 30 nm in width was directly observed, which was formed during the polarization reversal process. The presence of the step structure reveals that the forward domain-growth mechanism is the dominant domain-switching process in our PZT thin films. Received: 6 August 2002 / Accepted: 9 August 2002 / Published online: 28 October 2002 RID="*" ID="*"Corresponding author. Fax: +86-21/5241-3122, E-mail: huarongzeng@163.net     

Characterization of 90° domain structure and polarization switching in Pb(Zr0.4Ti0.6)O3 film by piezoresponse force microscope

A lead zirconate titanate Pb(Zr_0.4Ti_0.6)O₃ (PZT40/60) film was deposited on a Pt(111)/Ti/SiO₂/Si(100) substrate by a sol–gel process followed by thermal annealing at 650 °C for 5 min. Piezoresponse force microscope observation revealed a lamellar domain structure in the PZT40/60 grains and we attribute the lamellar domains as 90° ferroelectric domains. The polarization-switching mechanism of the 90° domains in the PZT40/60 film under external electric fields has also been studied and it was revealed that a large-area polarization switching is usually accompanied by the appearance of a new direction of 90° domains in order to reduce the stress in the grains. By contrast, a nanometer-sized polarization switching is believed to be accomplished by generating 180° domains within a single lamellar domain. PACS 77.80.-e; 77.84.-s; 68.55.-a; 68.37.-d     

外加电场对铁电薄膜相变的影响

采用热力学非线性理论,研究了外加电场对立方基底Pb(Zr_0.3Ti_0.7)O₃(PZT)铁电薄膜相变的影响.通过数值计算,得到了"失配应变-外加电场"相图,及外加电场与极化强度的关系.当外加电场达到186 kV/cm时,能使生长在SrTiO₃ 基底上PZT铁电薄膜从单斜r相转变为c相.在实验上,采用扫描探针显微镜通过对PZT薄膜施加不同的极化电场来研究了它的电畴翻转.从得到的压电响应相图可以看出,绝大多数的电畴是清晰可 关键词： 铁电薄膜 相变 扫描探针显微镜 失配应变     

Research on Raman-scattering and Fabrication of Multilayer Thin Film with Different Structures and Components Based on Pt/Ti/Si3N4/SiO2/Si Substrate

选用三水醋酸铅、乙酰基丙酮酸锆、四异丙氧基钛、乙酰丙酮作初始材料,用同样的方法分别制备了锆钛酸铅(PZT)和钛酸铅(PT)两种固体前驱物. 采用改良型的溶胶-凝胶工艺技术,分别在不同的Pt-Ti-Si₃N₄-SiO₂-Si基底上,按照不同的组合方式,制备了三种多层薄膜：PZT、PT/PZT-PZT/PT、PT/PZT/-/PZT/PT. 较详细地讨论了薄膜制备的工艺技术,发现当凝胶通过烧结和干燥后变成固态物质时,薄膜内部存在着较大的残余应力,当薄膜在600 ºC下退火时其内部残余应力可以被减小. 通过拉曼     

Lead telluride nanocrystalline thin films: Structure,optical characterization and a broadband dielectric spectroscopy study

Nanocrystalline PbTe thin films were deposited on a glass substrate by thermal evaporation technique with two thicknesses namely, 45 and 250 nm. The structural studies revealed that the films have nanocrystalline cubic structure and the particle size was found to be 11 and 20.7 nm, for low and high thicknesses respectively. The FE-SEM study shows that the surface grains increase for higher thickness film. This indicates that samples lying under the strong regime of confinement for PbTe thin films. The optical properties confirm the occurrence of confinement process as the optical band gap are 1.67 and 0.9 eV for 45 and 250 nm films, respectively. The dielectric results indicated that the conductivity increases by about two orders of magnitude with increasing the thickness from 45 to 250 nm. Moreover, the permittivity shows a higher dispersion step at lower frequencies in both samples due to the hopping conduction mechanism in addition to the interfacial polarization in such heterogeneous structures. Another small dispersion step is noticed in case of the lower thickness. It is attributed to the polarization of the accumulated charge carriers near the grain boundaries interfaces. No indication of any electrode phenomena in both samples is shown here.     

Enhanced energy storage behaviors in free-standing antiferroelectric Pb(Zr_(0.95)Ti_(0.05))O_3 thin membranes

Free-standing antiferroelectric Pb(Zr_(0.95)Ti_(0.05)O_3(PZT(95/5)) thin film is fabricated on 200-nm-thick Pt foil by using pulsed laser deposition.X-ray diffraction patterns indicate that free-standing PZT(95/5) film possesses an α-axis preferred orientation.The critical electric field for the 300-nm-thick free-standing PZT(95/5) film transiting from antiferroelectric to ferroelectric phases is increased to 770 kV/cm,but its saturation polarization remains almost unchanged as compared with that of the substrate-clamped PZT(95/5) film.The energy storage density and energy efficiency of the substrate-clamped PZT(95/5) film are 6.49 J/cm~3 and 54.5%,respectively.In contrast,after removing the substrate,the energy storage density and energy efficiency of the free-standing PZT(95/5) film are enhanced up to 17.45 J/cm~3 and 67.9%,respectively.     

Au/PZT/BIT/p-Si异质结的制备与性能研究

采用脉冲激光沉积(PLD)工艺,制备了以Bi₄Ti₃O₁₂(BIT)为过渡阻挡层的Au/PZT/BIT/p-Si异质结.研究了BIT铁电层对Pb(Zr_0.52Ti_0.48)O₃(PZT)薄膜晶相结构、铁电及介电性能的影响,对Au/PZT/BIT/p-Si异质结的导电机制进行了讨论.氧气氛530℃淀积的PZT为多晶铁电薄膜,与直接淀积在Si基片上相比,加入BIT铁电层后PZT铁 关键词： 铁电薄膜 异质结构 脉冲激光沉积(PLD)     

Thin-film capacitor M/Pb(ZrTi)O3/M as a polarization-sensitive photocell

A steady-state short-circuit photocurrent of preliminarily polarized submicron capacitors with a polycrystalline Pb(ZrTi)O₃ (PZT) film is investigated under irradiation by light with a wavelength λ > 0.4 μm. The structures with different M/PZT interfaces that differ in the leakage current by more than an order of magnitude are found to demonstrate virtually the same value of the photocurrent, which is always directed opposite to the ferroelectric polarization of the PZT film. Although the magnitude of photocurrent is determined by the degree of polarization of the film, the observed photocurrent is not a depolarization current of the ferroelectric film. Therefore, the M/PZT/M capacitor behaves like a polarization-sensitive photocell. Within the proposed theory of a heterophase medium, the dependence of the photocurrent on the magnitude of the preliminary polarization is calculated and proves to be in reasonable agreement with the experimental results.

     

Nd-Ce-Fe-B纳米复合薄膜的磁性及交换耦合作用

采用磁控溅射技术制备了具有永磁特征的Nd-Ce-Fe-B多层纳米复合薄膜,并对其进行了退火处理.通过改变退火温度,研究其对薄膜磁性能和晶体结构的影响.结果表明,随着退火温度的提高薄膜磁性能逐渐增大,但当温度达到695℃以上时,薄膜的磁性能急剧下降.当退火温度为675℃时,薄膜的矫顽力Hci=10.1 kOe(1Oe=79.5775 A/m),垂直于薄膜表面方向的剩余磁化强度4πM_(r⊥)=5.91 kG(1 G=10~3/(4π)A/m).薄膜的X射线衍射结果表明,磁性薄膜具有较好的c轴取向.通过对薄膜磁化反转过程的研究,发现随着外加磁场的增大,M_(rev)的极小值向M_(irr)减小的方向移动,这与畴壁弯曲模型类似,表明在薄膜中存在较强烈的局部钉扎作用,而剩余磁化强度曲线表明这种钉扎作用在薄膜矫顽力机制中并不占支配作用.此外,薄膜的Henkel曲线结果表明在薄膜中存在较强的交换耦合作用,在经过685℃退火的薄膜中磁相互作用更加显著.