铁电薄膜纳米尺度畴分布及其生长机制

用溶胶-凝胶的方法制得(111)取向的PZT铁电薄膜,并喷涂于Pt(111)/Ti/SiO2/Si衬底上.用扫描力显微镜(SFM)的压电响应模式纳米级分辨率地观察到了几乎等间距或中间间距大于两侧的条状畴结构.这主要与晶粒和衬底间的应力应变有关.从这畴结构我们提出铁电畴形核和生长速率模型.其基本过程如下(1)由于薄膜和底电极间周期性的结构和成分起伏,致使畴结构在此相连处形核.(2)铁电畴横向生长至相临畴相遇,纵向生长至薄膜上表面.(3)在随后的过程中,由于单个畴间的能量差异致使横向生长再次启动.这些过程是连续的,难以正确的区分.     

铁电材料的纳米尺度压电响应力显微术研究进展

压电响应力显微术是在原子力显微镜的基础上,利用材料自身逆压电效应来探测样 品表面形变的一类技术总称.现已作为铁电材料研究的重要手段,应用于纳米尺度畴结构的三 维成像、畴结构的动态研究、畴结构控制和微区压电、铁电、漏电等物理性能表征等领域.本 文就近年来利用压电响应力显微术对铁电材料的研究方面作一综述.     

计量型原子力显微镜环境温度的测控

在纳米结构的检测与表征领域中,温度是影响纳米尺度测量精度的重要误差源.为此,根据测量材料的热物性和空气折射率与光学测量的关系,以计量型原子力显微镜和大范围纳米测量机为例,首先通过设计高精度多点测温系统进行精密的温度测量,分析估计在扫描测量纳米结构过程中温度变化对其测量结果的影响.其次对纳米测昔中温度测量的相关技术问题进行了研究,以保证纳米表征和检测在纳米尺度及其量值上的准确性.     

采用计量型扫描力显微镜校准微纳米标准样板

为了建立质量保证体系,微米和纳米样板至今仍被广泛地应用于校准微纳米尺度的测量仪器中．介绍了应用由德国联邦物理研究所开发研究的、测量范围为25 mm×25 mm×5 mm的计量型扫描力显微镜(M-LRSFM)的校准方法．上述计量型扫描力显微镜配置有三个零拍的激光干涉仪,可分别测量沿x、y、z三条轴线方向的位移,因而其测量值可直接溯源于“米”定义．此种M-LRSFM能够校准横向的微纳尺度的结构尺寸,诸如阶梯高度、一维和二维光栅、镀层厚度、线宽、微纳尺度的表面粗糙度等．作为实例,介绍了一种横向样板的校准程序及获得的校准结果．研究表明这种方法适合于校验扫描电子显微镜(SEM)的放大倍率．     

O.92PZN-0.08PT晶体的缺陷与畴结构研究

应用环境扫描电子显微术(ESEM)、原子力扫描显微术(AFM)、同步辐射白光形貌术(SRWBT)等形貌成像技术研究了0.92PZN-0.08PT晶体的表面缺陷形态与铁电畴结构.通过对畴结构动态演化的同步辐射形貌观察,可揭示出该晶体的结构相变过程.     

苏州纳米所发表能源纳米器件的扫描力探针研究综述

<正>中科院苏州纳米所陈立桅研究员团队,长期致力于能源纳米器件界面形貌、化学结构和电子过程的扫描力探针研究。近日,受邀撰写综述文章聚焦近年来能源纳米器件的扫描力探针技术的研究进展。该综述首先介绍了扫描探针各种功能成像技术的发展历程,从最基本的形貌成像模式开始,依次介绍纳米力学模式,化学成像模式,载流子探测模式和时间分辨成像技术等。     

粗大晶粒PZT陶瓷中电畴的结构

应用扫描力显微镜(SFM)的压电响应模式观测未经抛光处理的PZT陶瓷片的电畴结构,用纵向压电响应信号和侧向压电响应信号获得PZT陶瓷材料三维电畴结构.结果表明,将样品晶粒的微形貌与SFM的纵向和侧向压电响应信号相结合,能准确表征粗大晶粒样品的三维电畴结构.用SFM可观测表面不经任何处理的陶瓷样品的电畴,不会引入表面应力等影响因素,能得到样品的原生畴结构.对原生畴结构的观察表明,对于受应力较大的晶粒,成畴的主要原因是降低应变能,而受应力较小的晶粒成畴的主要原因是降低退极化能.     

纳米声学及近场声成像技术

纳米声学是近年来迅速发展的新的学科领域,旨在亚微米和纳米尺度上来"听到"和"看到"我们尚未发现的物质世界。而近场声成像技术,像扫描探针声显微术(Scanning ProbeAcoustic Microscopy,SPAM)和压电响应力显微术(Piezoresponce Force Microscopy,PFM)等,不仅具有亚微米和纳米分辨力,而且能方便地对试样微区的表面形貌,材料的力学和电学等性质进行成像,是开展纳米声学研究的有效手段。文章结合实验结果,对SPAM和PFM等近场声成像技术作了简要介绍。     

瓦斯突出煤体的纳米结构研究方法

提出了一种研究瓦斯突出煤体的纳米结构的新方法,介绍了用原子力显微镜(AFM)对煤矿石进行扫描并得到高精度微观图像的实验过程.该方法基于AFM的纳米级分辨率,可清晰观测到煤的裂隙、孔隙等显微构造.除了显示煤样的纳米结构,AFM还可对样品成像进行多角度分析,用于煤中瓦斯气体的含量测定和煤层气的开发,以及瓦斯吸附机理和煤的微观特性的研究.     

纳米光学天线研究现状及进展

基于spp共振效应的纳米天线结构能有效收集光的能量,并将它限制在亚波长尺度,其巨大的局域场增强效应为纳米光子学大范围的应用提供了广阔的前景,例如,纳米尺度内光信息的处理和传播、近场显微镜超分辨率成像、高效太阳能电池、超高密度近场光存储、纳米光刻、量子单光予源、高效率纳米电磁波集中器、高灵敏度生化传感器等。文章在介绍纳米天线的基本构造和工作原理的基础上,综述了其在多个领域的应用。     

Three-dimensional observation of nanoscale ferroelectric domains using scanning nonlinear dielectric microscopy with electric field correction by Kelvin probe force microscopy

An advanced technique for the measurement of three-dimensional ferroelectric domain structure is described. Scanning nonlinear dielectric microscopy is used to measure the polarization components both perpendicular and parallel to the specimen surface. A nanoscale electric field correction is devised and performed using Kelvin probe force microscopy to allow more precise measurement of the nanoscale polarization component parallel to the specimen surface. Using this electric field correction, three-dimensional imaging of the ferroelectric polarization orientation is demonstrated.     

Non-volatile domain nucleation and growth in multiferroic BiFeO3 films

We have presented a systematical study of the domain nucleation and growth behaviors in multiferroic BiFeO(3) (BFO) films. Both the ferroelectric and the ferroelastic switching dynamics were investigated. Several environmental parameters, including the polarization orientations, the monodomain-like matrix, and the ordered domain walls as local boundaries, were well controlled by thin-film strain engineering through changing the vicinal angles of the substrates. The tip-based domain dynamics was studied by subsequent piezoresponse force microscope (PFM) imaging of the domain evolution under external voltage pulses. For the nanodomains written in the monodomain-like environment, the domain wall performed the thermal activated motion. The as-grown 71° domain walls can act as pinning centers for the ferroelectric domain growth driven by low fields; moreover, ferroelastic nucleation near a 71° domain wall will cause the deformation of the domain wall. The ferroelastic domain growth possessed relatively small activation fields, and therefore usually performed non-activated motion. This study revealed the effects of local environments on the dynamics forming nanoscale domains, and opened a pathway for applications in novel non-volatile functional devices.     

Near-field acoustic and piezoresponse microscopy of domain structures in ferroelectric material

Three kinds of near-field microscopy imaging mode including SEAM (Scanning electron acoustic microscopy), PFM (Piezoresponse force microscopy) and SPAM (Scanning probe acoustic microscopy) have been developed to investigate domain structures of ferroelectric ceramics, crystals and thin films in our studies. The domain imaging mechanisms are presented individually in three imaging modes. Sub-surface micro-domain configuration of ferroelectric BaTiO₃ ceramics and single crystal and their dynamic behavior under external fields were clearly visualized by SEAM. Ferroelectric domain structures of ferroelectric PZT thin film and PMN-PT single crystal were characterized by PFM. Nanoscale switching behavior and local field-induced nanoscale displacement behavior of domain structures in ferroelectric thin film were studied by PFM. Antiparallel domain patterns in ferroelectric transparent PLZT ceramics were also characterized by SPAM. The combination of SEAM, PFM and SPAM in application to imaging domain structures undoubtedly enrich our understanding of the nature of piezoelectricity and ferroelectricity at submicro-, even nano-meter scale.     

Spontaneous vortex nanodomain arrays at ferroelectric heterointerfaces

The polarization of the ferroelectric BiFeO(3) sub-jected to different electrical boundary conditions by heterointerfaces is imaged with atomic resolution using a spherical aberration-corrected transmission electron microscope. Unusual triangular-shaped nanodomains are seen, and their role in providing polarization closure is understood through phase-field simulations. Heterointerfaces are key to the performance of ferroelectric devices, and this first observation of spontaneous vortex nanodomain arrays at ferroelectric heterointerfaces reveals properties unlike the surrounding film including mixed Ising-Ne?el domain walls, which will affect switching behavior, and a drastic increase of in-plane polarization. The importance of magnetization closure has long been appreciated in multidomain ferromagnetic systems; imaging this analogous effect with atomic resolution at ferroelectric heterointerfaces provides the ability to see device-relevant interface issues. Extension of this technique to visualize domain dynamics is envisioned.     

Piezoresponse force microscopy studies of nanoscale domain structures in ferroelectric thin film

Piezoresponse force microscopy was used to perform studies of nanoscale domain imaging, limit of ferroelectric nano-sized grains and electric field-induced displacement behavior of domain structures in ferroelectric PZT thin film. Nanoscale 180° and 90° domain configurations as small as 30 nm in size were clearly visualized in the individual grains. It was demonstrated that domain configuration was strongly dependent on the size of the grains. The limit of ferroelectric nano-sized grains was found to be smaller than 25 nm. Nanoscale displacement versus field hysteresis loops were obtained in ferroelectric domains of PZT thin film, and discussed in terms of phenomenological theory.     

A decade of piezoresponse force microscopy: progress, challenges, and opportunities

Coupling between electrical and mechanical phenomena is a near-universal characteristic of inorganic and biological systems alike, with examples ranging from piezoelectricity in ferroelectric perovskites to complex, electromechanical couplings in electromotor proteins in cellular membranes. Understanding electromechanical functionality in materials such as ferroelectric nanocrystals and thin films, relaxor ferroelectrics, and biosystems requires probing these properties on the nanometer level of individual grain, domain, or protein fibril. In the last decade, piezoresponse force microscopy (PFM) was established as a powerful tool for nanoscale imaging, spectroscopy, and manipulation of ferroelectric materials. Here, we present principles and recent advances in PFM, including vector and frequency-dependent imaging of piezoelectric materials, briefly review applications for ferroelectric materials, discuss prospects for electromechanical imaging of local crystallographic and molecular orientations and disorder, and summarize future challenges and opportunities for PFM emerging in the second decade since its invention     

Advanced fabrication and characterization of epitaxial ferroelectric thin films and multilayers

Understanding the behavior of ferroelectrics on the nanoscale level requires the production of materials of the highest quality and advanced characterization techniques for probing the fascinating properties of these systems with reduced dimensions. Here we give an overview of our recent achievements in this area, which includes the detailed study of the suppression of ferroelectricity in PbTiO3 thin films, the fabrication of PbTiO3/SrTiO3 superlattices in which ferroelectricity shows some surprising behavior, and finally the manipulation of nanoscale ferroelectric domains using the atomic force microscope which leads to the precise analysis of domain wall creep and roughness in Pb(Zr,Ti)O3 thin films.     

Nanoscale ferroelectric field-effect writing and reading using scanning tunnelling spectroscopy

Control of the density of mobile charge carriers using electric fields is widely used in a variety of metal-insulator-semiconductor structures and is the governing principle behind the operation of field-effect transistors. Ferroelectric materials possessing a switchable and non-volatile polarization field can be used as insulating layers, revealing new opportunities for device applications. Advances in material processing and in particular complex oxide thin-film growth mean that high-quality field-effect devices can be based on ferroelectric/metallic oxide heterostructures. In addition, advances in local probe techniques such as atomic force microscopy allow them to be used in the imaging and study of small ferroelectric domain structures in bulk crystals and thin films. Meanwhile, scanning tunnelling microscopy and spectroscopy have established themselves as powerful techniques for atomic manipulation and nanometre-resolution electron tunnelling spectroscopy. Here, a scanning tunnelling microscope is used to investigate the ferroelectric field effect in all-perovskite heterostructures. Scanning tunnelling spectroscopy allows us to probe the local electronic properties of the polarized channel of a ferroelectric field-effect device as a function of the field orientation. This technique can be used to read and write ferroelectric field-induced regions with a size as low as 20 nm.     

Piezoresponse force microscopy and recent advances in nanoscale studies of ferroelectrics

In this paper, we review recent advances in piezoresponse force microscopy (PFM) with respect to nanoscale ferroelectric research, summarize the basic principles of PFM, illustrate what information can be obtained from PFM experiments and delineate the limitations of PFM signal interpretation relevant to quantitative imaging of a broad range of piezoelectrically active materials. Particular attention is given to orientational PFM imaging and data interpretation as well as to electromechanics and kinetics of nanoscale ferroelectric switching in PFM.