Analysis of polarization switching in ferroelectric crystals in the injection mode

We report on the results of experiments on polarization switching in a ferroelectric TGS crystal during injection of electron beams from a scanning electron microscope under a surface layer. A series of models reflecting the polarization switching dynamics of a ferroelectric crystal under the action of an injected charge is constructed. The implementation of these models is based on the principles of evolution of domain structures taking into account analysis of possible polarization switching mechanisms for ferroelectric samples. A mathematical model developed using these principles demonstrates qualitative similarity of model current pulses and those obtained experimentally in the injection mode.     

Investigation of the fractal features of the polarization reversal processes in ferroelectric crystals under injection conditions

The features of polarization reversal processes of ferroelectric crystals are analyzed under the condition that electron beams of a scanning electron microscope are injected into the subsurface layer of a sample. The proposed mathematical model describes the dynamics of the polarization switching of a ferroelectric crystal using the injection contact technique. The simulation relies on the basic principles of scale invariance in domain structure evolution. The polarization switching current of ferroelectric crystals is investigated as the dynamic characteristic of a finite medium exhibiting fractal behavior. The application of fractal and multifractal analysis of a time series enables us to calculate the fractal dimension of the polarization reversal process under injection conditions.     

Periodic domain structure in Czochralski-grown LiNbO3: Y crystals

A study is reported of the correlation between the impurity distribution and the ferroelectric domain structure in a periodically polarized LiNbO₃: Y crystal grown by the Czochralski method. The domain walls forming near the impurity concentration modulation extrema are shown to be shifted by the temperature gradient below the Curie point. A new positive domain was observed to form near the trace of an electron beam scanning the $\{ 01\bar 10\} $ crystal surface in the course of x-ray microprobe analysis.     

Electret states and the phase transition in a surface layer of the TlGaSe2 ferroelectric semiconductor

The electret polarization is investigated in the TlGaSe₂ ferroelectric semiconductor. It is proved for the first time that stable internal electric fields associated with residual electret polarization are induced in crystals of the TlGaSe₂ ferroelectric semiconductor at temperatures T < 200 K. It is experimentally established that the peak of the pyroelectric current measured in the vicinity of the phase transition to the ferroelectric polar phase depends substantially on the temperature at which the external electric field is switched off when the TlGaSe₂ ferroelectric crystal under investigation is preliminarily cooled from room temperature. The results obtained are discussed in the framework of a model according to which internal electret fields are induced by charges localized at different levels in the bulk and on the surface of the TlGaSe₂ ferroelectric crystal. These fields drastically change at temperatures in a narrow range near 135 K. The inference is made that a phase transition occurs in the surface layer of the TlGaSe₂ crystal at a temperature close to ～135 K.     

Potential relief on the surface of polarized ferroelectric electrets from an analysis of the anomalous electron emission spectra

A technique is proposed for determining the specific features in the potential distribution over a free surface of polarized ferroelectric electrets from analyzing the anomalous electron emission spectra. This technique is applied to examine the potential distribution over the surface of a lead magnoniobate single crystal and ferroelectric ceramics. Reasoning from the results obtained for the lead magnoniobate crystal, the inference is drawn that the degree of perfection of surface layers of ferroelectric single crystals can be controlled using the anomalous electron emission spectra.     

Kinetics of electron emission from the TGS ferroelectric crystal

A study is reported on the behavior in time of the electron emission current density from a triglycine sulfate ferroelectric crystal measured at fixed temperatures. This relation is shown to have an exponential nature. The characteristic emission relaxation time depends on temperature and decreases as one approaches the phase-transition point. The magnitude of the relaxation time and its temperature dependence can be accounted for both within a mechanism in which the emission decay is associated with the emptying of surface electron states, and in terms of the Maxwellian relaxation process.     

Physical and mathematical modeling of the electron-beam-induced charging of ferroelectrics during the process of domain-structure switching

The results of modeling the dynamic charging processes that arise when ferroelectrics are under the action of an electron beam in a scanning electron microscope are presented. Implementation of the model is based on simultaneous solution of the continuity equation and Poisson equation with allowance for the radiation-stimulated intrinsic conductivity of the irradiated sample and with an initial charge distribution determined using the Monte Carlo method. The multidimensional boundary evolutionary problem is solved using grid methods. The model permits one to study the dynamics of the process of the electron-beam-induced charging of ferroelectrics. Estimates for the values of fields generated by charges accumulated during the irradiation process are presented for a set of modeling parameters corresponding to physical data obtained in experimental observations of the polarization switch for a ferroelectric lithium niobate crystal.     

Simple macroscopic model of pyroelectric phenomenon in TGS single crystals in ferroelectric phase

A simple mathematical model of pyroelectric phenomena, for ideal ferroelectrics, is presented. Material constants for triglycine sulphate (TGS) are used to verify the model. The results of simulations were compared with the temperature characteristics of the pyroelectric coefficient measured for a TGS ferroelectric sample. Single crystal growth and preparation of samples and experimental procedure are also presented. The relatively good conformity of the model calculations with the measurements allow us to expect further useful application of the model in future work on ferroelectric single crystals.     

Annealing effect of platinum-based electrodes on physical properties of PZT thin films

This study examined the crystal structure and surface morphology, including the Ti segregation mechanism on the surface due to the inter-diffusion between Pt, Ti and TiO_x as a glue layer, according to the annealing temperature and growth orientation of a Pt film. In addition, the fatigue mechanism of ferroelectric PZT thin films deposited on a Pt-based electrode was also investigated. The nano-structure, orientation mapping, and micro-morphologies of the triangular Pt hillocks were investigated by scanning electron microscopy with an electron backscatter diffraction (EBSD) function. The D–E hysteresis loop of the ferroelectric films was measured using a Sawyer–Tower circuit at 1 kHz to obtain the remanent polarization and coercive field.     

Observation of Ferroelastic and Ferroelectric Domains in AgNbO_3 Single Crystal

Compared to AgNbO_3 based ceramics, the experimental investigations on the single crystalline AgNbO_3, especially the ground state and ferroic domain structures, are not on the same level. Here, based on successfully synthesized AgNbO_3 single crystal using a flux method, we observed the coexistence of ferroelastic and ferroelectric domain structures by a combination study of polarized light microscopy and piezoresponse force microscopy.This finding may provide a new aspect for studying AgNbO_3. The result also suggests a weak electromechanical response from the ferroelectric phase of AgNbO_3, which is also supported by the transmission electron microscope characterization. Our results reveal that the AgNbO_3 single crystal is in a polar ferroelectric phase at room temperature, clarifying its ground state which is controversial from the AgNbO_3 ceramic materials.     

聚合物网络稳定铁电液晶中的条纹织构的研究

对聚合物网络稳定的铁电液晶体系进行了研究.实验表明,在聚合物网络单体聚合过程中施加低频交变电场，在偏光显微镜下观察到均匀的液晶分子排列出现一新的条纹织构.从体系自由能的角度对条纹织构给出合理的解释. 关键词：     

Electron holography with atomic focusers

In a modified form of electron holography, as originally proposed by Gabor, a specimen illuminated by the focused, convergent beam of a scanning transmission electron microscope is followed by a thin crystal which acts as a periodic array of atomic focusers. Each of the broad diffraction spots of the crystal then contains a magnified image of the specimen with a resolution limit of 0.05 nm or less. The method is illustrated by images of crystal lattice planes and tungsten atoms in the diffraction patterns formed by crystals in the walls of carbon nanoshells.     

聚合温度及铁电液晶有序度对单体转化率的影响

采用琉醇和丙烯酸的混合物作为反应单体,利用红外光谱仪检测反应前后单体的C=C双键吸收峰的变化,研究了温度对单体转化率的影响。制备了单体含量为10%的聚合物稳定铁电液晶器件,研究了铁电液晶有序度对单体的影响。实验表明:随着温度的增加单体的转化率增加,随着铁电液晶有序度的增加单体的转化率增加;在铁电液晶中单体的转化率主要受有序度的影响;制备聚合物稳定铁电液晶器件最佳的聚合条件为近晶A相(SmA)下聚合。     

Thermally stimulated electron emission in the paraelectric phase of triglycine sulfate crystals heated at a high rate

Thermally stimulated electron emission is experimentally observed in ferroelectric triglycine sulfate (TGS) crystals in a temperature range whose upper limit is 10–15 K above the Curie point. Samples of a nominally pure and a chromium-doped TGS crystal, heated at different constant rates q=dT/dt, are investigated. It is shown that an increase in the heating rate results in increased emission current density over the entire temperature range investigated. The temperature at which emission arises depends only slightly on the rate q. At the same time, the temperature at which emission ceases increases monotonically with increasing q; if q is less than 1 K/min, this temperature is below the Curie point, while at q=4–5 K/min, this temperature becomes as large as 60–65°C, which is more than 15°C above the Curie point. In chromium-doped TGS crystal, the electron emission onset temperature is close to that of pure TGS, but the width of the temperature range over which emission is observed in the paraelectric phase is approximately two times less than in the case of pure TGS heated at the same rate. The emission disappearance below the Curie point (in the ferroelectric phase) at low q is explained as a result of full emptying of the electron traps under slow heating. The reason for the occurrence of emission above the Curie point is related to the charges that shield the spontaneous polarization and, because of their slow relaxation, persists in the paraelectric phase.     

Visualization of field induced ferroelectric electron emission from TGS using emission electron microscopy

Field induced electron emission from triglycinesulfate (TGS) has been investigated using parallel imaging electron emission microscopy (EEM). The emission phenomenon has been induced by applying an ac electrical field up to 2 kV/mm to a single crystal of approximately 0.1 mm thickness. Emission patterns have been observed as a function of the applied field amplitude and of the crystal temperature. At voltages below the coercive field, no emission is visible. When approaching the Curie temperature, emission gradually disappears. This indicates an electron emission mechanism relying on the existence of a switchable ferroelectric phase. The information content of the images is discussed, an interpretation is given on the basis of existing theories. PACS 68.37.-d; 77; 77.80.Fm; 77.80.-e     

SEM扫描云纹法的相移技术研究

提出一种扫描电镜(SEM)扫描云纹法的相移新技术,通过SEM系统控制电镜电子束扫描线移动,对获取的云纹图像实现0-2π范围内的四步相移,从而获得了更高的位移测量灵敏度。同时对SEM扫描云纹法的测量原理以及相移实验技术的原理进行了详细的阐述。并将该技术应用到电子封装试件栅的相移分析中。实验结果证明了该方法的可行性,该方法为微米云纹法的条纹处理提供了一种新途径。     

Dynamic magnonic crystal based on a layered ferrite–ferroelectric structure

A dynamic magnonic crystal based on a planar multiferroid ferrite–ferroelectric structure is suggested and studied. A space-periodic electric field applied to the ferroelectric layer converts a regular multi-ferroid waveguide to a periodic structure. An electrodynamic model of a dynamic magnonic crystal is constructed, and its dispersion and transfer characteristics are studied.     

Microscopic origin of the giant ferroelectric polarization in tetragonal-like BiFeO(3)

We report direct experimental evidence for a room-temperature, ～130 μC/cm(2) ferroelectric polarization from the tetragonal-like BiFeO(3) phase. The physical origin of this remarkable enhancement of ferroelectric polarization has been investigated by a combination of x-ray absorption spectroscopy, scanning transmission electron microscopy, and first principles calculations. A large strain-induced Fe-ion displacement relative to the oxygen octahedra, combined with the contribution of Bi 6s lone pair electrons, is the mechanism driving the large ferroelectric polarization in this tetragonal-like phase.     

Estimation of SEM imaging resolution of the domain structure of pyroprobe-heated ferroelectrics

The specific contrast of scanning electron microscope (SEM) images of ferroelectric domains observed in the pyrocurrent (pyroprobe) mode is analyzed. Calculations taking into account both the nonuniform heating of domains and the heat diffusion via the domain walls and the crystal boundaries are performed. It is established that the heat diffusion smears the domain images of small domains. Along with the probe diameter, the scan rate is shown to be an important factor determining the character of the SEM image contrast. A decrease in the scan rate may appreciably lower the resolution even in case of a fairly thin probe.     

聚(偏氟乙烯-三氟乙烯)纳米薄膜极化反转与疲劳特性

采用旋涂法制备了厚度为140 nm的聚(偏氟乙烯-三氟乙烯)[P(VDF-TrFE)]纳米薄膜, 研究了不同退火温度以及环境相对湿度对薄膜的极化反转和疲劳性能的影响. 运用X射线衍射仪、扫描电子显微镜和傅里叶变换红外光谱仪等测试技术对薄膜的微结构进行了表征. 实验结果表明, 通过不同温度的退火处理, P(VDF-TrFE)铁电薄膜的结晶度随着退火温度的升高而不断提高, 并且一定的温度范围内的退火处理可以提高薄膜的极化性能; 此外, P(VDF-TrFE) 铁电薄膜性能还表现出一定的环境湿度的敏感特性, 这与薄膜的物理性能和结构特点密切相关; P(VDF-TrFE)铁电薄膜在不同的环境湿度条件下 表现出较好的电学特性, 其漏电流均保持在10 ^-7A/cm² 的较低水平. 本工作揭示了再退火过程对薄膜的极化反转速度和疲劳恢复特性的影响, 并结合薄膜二次疲劳结果, 探讨了薄膜可逆的内部疲劳恢复特性机理.