Electrostatic force microscopy study on the domain switching properties of the Pb(Zr0.2Ti0.8)O3 thin films with different crystallographic orientations for the probe-based data storage

The domain switching properties of the ferroelectric Pb(Zr_0.2Ti_0.8)O₃ (PZT) thin films with two types of crystallographic orientations were investigated by electrostatic force microscopy (EFM). The crystallographic orientations of the PZT thin films were random on the (1 1 1)Pt/MgO(1 0 0) and c-axis preferred on the (1 0 0)Pt/MgO(1 0 0), respectively. When dc bias was applied to the films for writing in micro-scale area, electrostatic force images showed that the domain switching was hard in the PZT thin films with random orientation, while the pattern could clearly be written in the PZT films with c-axis orientation. The differences in the domain switching properties of each PZT thin film were investigated in the crystallographic orientations point of view, and the domain switching dynamics were also measured by investigating the nano-sized dot switching behavior with respect to the width of the applied voltage pulse.     

Study on the c-axis preferred orientation of ZnO film on various metal electrodes

ZnO thin film was deposited on various metal electrodes by reactive sputtering, and c-axis preferred orientation of the film has been studied. ZnO, which has high piezoelectricity, is promising for oscillators or filter devices such as surface acoustic wave (SAW) device, gas sensor, and film bulk acoustic resonator (FBAR). But, for the application of ZnO film for these devices, the film should be grown with c-axis normal to the electrode. In this study, Pt, Al, and Au were deposited on Si wafer, and the surface roughness and crystal structure of the ZnO film on the electrode were investigated using AFM, scanning electron microscopy (SEM), and X-ray diffraction (XRD). Columnar structures of ZnO films were grown with c-axis normal to all electrodes, and among them Pt electrode showed the highest preferred orientation of ZnO film.     

Characterization of lead zirconate titanate--lanthanum ruthenate thin film structures prepared by chemical solution deposition

In this work, the results of compositional and microstructural analysis of lead zirconate titanate--lanthanum ruthenate thin film structures prepared by chemical solution deposition are discussed. The cross-section transmission electron microscope (TEM) micrographs of the La-Ru-O film deposited on a SiO2/Si substrate and annealed at 700 degrees C revealed RuO2 crystals embedded in a glassy silicate matrix. When the La-Ru-O film was deposited on a Pt/TiO2/SiO2/Si substrate, RuO2 and La4Ru6O19 crystallized after annealing at 700 degrees C. After firing at 550 degrees C randomly oriented lead zirconate titanate (PZT) thin films crystallized on the La-Ru-O/SiO2/Si substrate, while on La-Ru-O/Pt/TiO2/SiO2/Si substrates PZT thin films with (111) preferred orientation were obtained. No diffusion of the Ru atoms in the PZT film was found. Ferroelectric response of PZT thin films on these substrates is shown in comparison with the PZT film deposited directly on the Pt/TiO2/SiO2/Si substrate without a La-Ru-O layer.     

Dynamics of space and polarization charges of ferroelectric thin films measured by atomic force microscopy

Retention behavior and local hysteresis characteristics in Pb(Zr(0.52)Ti(0.48))O(3) (PZT) thin films on Pt electrodes have been investigated by electrostatic force microscopy (EFM). A sol-gel method is used to synthesize PZT thin films and drying conditions are carefully explored over a wide range of temperature. Decay and retention mechanisms of single-poled and reverse-poled regions of the ferroelectric thin films are explained by space charge redistribution. Trapping behavior of space charges is dependent on the nature of interface between ferroelectric thin films and bottom electrodes. Local measurement of polarization-electric field curves by EFM shows inhomogeneous space charge entrapment.     

厚度效应对Pb(Zr0.53Ti0.47)O3薄膜微结构、铁电、介电性能的影响

用改进的溶胶-凝胶法在Pt(111)/Ti/SiO₂/Si(100)衬底上制备了不同厚度的高度(111)取向的Pb(Zr_0.53Ti_0.47)O₃薄膜.运用X射线衍射(XRD)和原子力显微镜(AFM)分析了薄膜的微结构,原子力显微镜表明厚度为0.3μm和0.56μm的PZT薄膜的晶粒尺寸和表面粗糙度分别为0.2～0.3μm、2～3μm和0.92nm、34nm.0.3μm和0.56μm PZT薄膜的剩余极化(Pr)和矫顽场(Ec)分别为32.2μC/²、79.9kV/cm, 27.7μC/cm²、54.4kV/cm;在频率100KHz时,薄膜的介电常数和介电损耗分别为539、0.066,821、0.029.     

Influence of substrate orientation on the morphologyand orientation of LaNiO3 thin films

LaNiO₃ thin films were successfully prepared by a chemical method from citrate precursors. The LNO precursor solution was spin‐coated onto Si (100) and Si (111) substrates. To obtain epitaxial or highly oriented films, the deposited layers were slowly heated in a gradient thermal field, with a heating rate of 1° min^?1, and annealed at 700°C. The influence of different substrate orientations on the thin film morphology was investigated using atomic force microscopy and X‐ray diffraction analysis. Well‐crystallized films with grains aligned along a certain direction were obtained on both substrates. Films deposited on both substrates were very smooth, but with a different grain size and shape depending on the crystal orientation. Films deposited on Si (100) grew in the (110) direction and had elongated grains, whereas those on Si (111) grew in the (211) direction and had a quasi‐square grain shape.     

A study of the initial growth of PtxCo(1−x) thin films on Si3N4

Pt _x Co_{(1− x )} thin films where x  =0.24 have been deposited onto Si₃N₄ windows and studied using transmission electron microscopy. The films are used in ultrahigh-density recording studies and it was found that the surface of the substrate had a strong influence on the microstructure, crystallography and magnetic properties of the film. An investigation of the early growth of the film was made by studying films of different thickness between 100 and 300 Å. It was found that the grains were hexagonal in structure with a strong c -axis orientation perpendicular to the surface.     

The charge storage characteristics of PZT nanocrystal thin film

Lead zirconate titanate (PZT) films have been extensively investigated for many applications: the nonvolatile memory devices based on their remarkable ferroelectric properties, the microelectromechanical system (MEMS) based on their piezoelectricity as well in sensors as in actuators. In this paper, we inject charges into PZT thin films, and then the charge storage and transportation through PZT thin films were observed by electric force microscopy (EFM). Results were studied and charging mechanisms were proposed.     

Piezoelectric and electromechanical properties of relaxor ferroelectric Pb(Mg1/3Nb2/3)O3(65%)-PbTiO3(35%) thin films observed by scanning force microscopy

Relaxor ferroelectric PbMg(1/3)Nb(2/3)O(3)(65%)-PbTiO(3)(35%) (PMN-35PT) thin films were grown by a sol-gel method on Pt(111)/TiO(2)/SiO(2)/Si(100) substrates. Piezoresponse and poling behavior appear to have a relation with the relaxor behavior of the materials. Piezoelectric images were studied in a number of regions on the films with subsequent statistical analysis of the obtained data using the contact mode of scanning force microscopy. Hysteresis loops were observed with external field applied over a wide range of the vibration frequency. The piezoelectric coefficient, d(33), and the crystallographic electrostrictive constant, Q(33), were also determined as 100pm/V and 2.8x10(-3)C(-2)m(4), respectively.     

A crystalline test specimen for checking the performance of high-resolution electron microscopes

A thin single crystal (001) film of gold with a favourable perforation is described. Examples of its versatile applications to test procedures and calibrations in high-resolution electron microscopy are illustrated. The advantage of such gold films mainly results from the good visibility of dark-field/bright-field image displacements at perforation edges in well defined crystallographic orientations.     

磁过滤阴极弧法TiN薄膜的制备及其微观机械性能研究

采用“S”型磁过滤阴极弧等离子体沉积技术,室温下在（111）面单晶硅上沉积氮化钛薄膜。采用AFM和XRD技术分别对薄膜的表面形貌和晶体择优取向进行了表征,并用微刻划的方法分析薄膜的微观机械性能。结果表明,薄膜表面光滑致密,随偏压的增大,表面颗粒粒径先增大后减小,并且从（111）面的择优取向转变成（220）面。在刻划实验中,随载荷增加,薄膜先后经历了完全弹性变形,弹-塑性变形和脆性断裂阶段。利用直接和间接2种方法对得到的薄膜的临界载荷进行分析对比,发现在不同负偏压下,薄膜的内应力和临界载荷不同。随着负偏压的增大,薄膜的内应力逐渐增大,临界载荷逐渐减小。在-100V偏压下制备的氮化钛薄膜的微观机械性能最为理想。     

Characterization of self-assembling isolated ferroelectric domains by scanning force microscopy

Lead zirconate titanate (PZT) thin films were prepared by a sol–gel process on platinized Si substrate. Their microstructure and surface morphology were characterized by XRD and Scanninn Force Microscopy. Phase transformation of the prepared PZT films from pyrochlore to ferroelectric was observed by XRD and PFM (piezoresponse force microscopy), respectively. Self-assembling nano-structured ferroelectric phases are fabricated by solution deposition technique followed by the controlling kinetics of the transformation. Complex structures of ferroelectric domains in the isolated ferroelectric phases were found in the furnace annealed PZT films in the temperature range of 400–500°C. Single ferroelectric domain structure in the isolated ferroelectric phases could be found in thinner PZT films and used to study the size effect of laterally confined ferroelectric domains.     

硅基PZT压电功能结构研究

PZT压电薄（厚）膜是制备MEMS传感元件和执行元件重要的功能材料,对近年PZT薄（厚）膜在MEMS领域的研究现状进行了分析,提出了一种新型的双杯PZT/Si膜片式功能结构;采用有限元方法对双杯PZT/Si膜片进行了结构优化,得到PZT和上、下硅杯的结构优化值为DPZT: D1:D2 =0.75:1.1:1;一阶模态谐振频率为13.2KHz;以氧化、双面光刻、各向异性刻蚀,以及PZT厚膜丝网印刷等工艺技术制作了双杯硅基PZT压电厚膜膜片,该膜片具有压电驱动功能。双杯PZT/Si膜片式功能结构的MEMS技术兼容性好,对芯片内其它元件或电路的影响小,适合作为MEMS片内执行元件的驱动机构。     

基于二维光学相干层析的多层薄膜结构无损定量评价

为了实现对多层薄膜结构厚度进行快速准确的测量和无损定量评价,研制了二维光学相干层析(Optical Coherence Tomography,OCT)系统,避免了传统一维OCT系统逐点扫描导致成像效率低下的问题。阐述了去除OCT共轭镜像理论,采用了五步相移干涉法,具体由压电驱动器驱动参考镜实现,做到了对OCT共轭镜像的去除,避免出现OCT图像的混叠。所研制的OCT系统具有极高的系统分辨率和较好的信噪比,可以实现对手机钢化玻璃薄膜内部四层结构厚度(钢化玻璃、静电胶层1、防爆贴膜和静电胶层2)进行准确测量。实验结果表明:自研制的系统可快速高精度地对多层薄膜结构厚度进行测量,可以推荐使用在多层薄膜的无损定量评价中。     

Development of RF magnetron sputtering method to fabricate PZT thin film actuator

PZT piezoelectric very thin films suitable for a microactuator have been deposited onto Invar alloy substrate using a high-temperature RF magnetron sputtering technique. PZT thin films must be deposited onto conductive substrate for a monomorph or a bimorph actuator. The chemical composition and the crystalline structure of these films were measured by ESCA and XRD, respectively. The chemical composition of PZT deposited stoichiometrically was almost the same as commercially-produced bulk PZT. Crystal planes (1 1 0) and (1 1 1) of PZT perovskite structure were observed in XRD analysis. When the substrate was heated to above 600 °C, SEM revealed only a very small number of pinholes on the surface. A thin (500 nm) film actuator has been characterized by measuring the piezoelectric property using a Laser Doppler Vibrograph. It was confirmed that the piezoelectric property has a linear relationship with the grain size, which also increased with the substrate temperature. The piezoelectric property of deposited PZT thin films showed a good agreement with a quoted value of bulk PZT, when the substrates were heated to 600 °C.     

静电辅助气溶胶化学气相沉积法制备Al_2O_3薄膜

以乙酰丙酮铝为前驱体,N,N-二甲基甲酰胺为溶剂,采用静电辅助的气溶胶化学气相沉积(ESAVD)方法,在Si(100)衬底上制备了Al2O3薄膜,并采用场发射扫描电镜、能谱仪、X射线衍射仪和自动划痕仪等设备对制备的薄膜进行了表征。结果表明:采用ESAVD法制备的Al2O3薄膜平整致密而且晶粒细小,薄膜与基体之间及薄膜内部都未出现开裂现象;薄膜与基体的结合力约为5.56 N;沉积得到的薄膜为化学计量比为2∶3的氧化物薄膜;退火前的薄膜为非晶态,在1 200℃退火保温2 h后薄膜转变为-αAl2O3。     

Calorimetry of epitaxial thin films

Thin film growth allows for the manipulation of material on the nanoscale, making possible the creation of metastable phases not seen in the bulk. Heat capacity provides a direct way of measuring thermodynamic properties of these new materials, but traditional bulk calorimetric techniques are inappropriate for such a small amount of material. Microcalorimetry and nanocalorimetry techniques exist for the measurements of thin films but rely on an amorphous membrane platform, limiting the types of films which can be measured. In the current work, ion-beam-assisted deposition is used to provide a biaxially oriented MgO template on a suspended membrane microcalorimeter in order to measure the specific heat of epitaxial thin films. Synchrotron x-ray diffraction showed the biaxial order of the MgO template. X-ray diffraction was also used to prove the high quality of epitaxy of a film grown onto this MgO template. The contribution of the MgO layer to the total heat capacity was measured to be just 6.5% of the total addenda contribution. The heat capacity of a Fe(.49)Rh(.51) film grown epitaxially onto the device was measured, comparing favorably to literature data on bulk crystals. This shows the viability of the MgO∕SiN(x)-membrane-based microcalorimeter as a way of measuring the thermodynamic properties of epitaxial thin films.     

Study on the c-axis preferred orientation of ZnO film on various metal electrodes

ZnO thin film was deposited on various metal electrodes by reactive sputtering, and c-axis preferred orientation of the film has been studied. ZnO, which has high piezoelectricity, is promising for oscillators or filter devices such as surface acoustic wave (SAW) device, gas sensor, and film bulk acoustic resonator (FBAR). But, for the application of ZnO film for these devices, the film should be grown with c-axis normal to the electrode. In this study, Pt, Al, and Au were deposited on Si wafer, and the surface roughness and crystal structure of the ZnO film on the electrode were investigated using AFM, scanning electron microscopy (SEM), and X-ray diffraction (XRD). Columnar structures of ZnO films were grown with c-axis normal to all electrodes, and among them Pt electrode showed the highest preferred orientation of ZnO film.     

Patterned crack-free PZT thick films for micro-electromechanical system applications

The fabrication and structuring of multilayer-thick film piezoelectric (PZT-lead zirconate titanate) structures, using composite sol-gel techniques and wet etching is described. The composite sol-gel technique involves producing a PZT powder/sol composite slurry which when spun down, yields films a few micrometres thick. Repeated layering and infiltration has been used to produce PZT films between 10 and 40 μm thick. Due to the low firing temperature (<720°C), it has also been possible to produce PZT films with embedded thin (ca. 100 nm thick) metal electrodes. The PZT thick films have also been structured using a wet etching technique. Examples of features and cavities with lateral dimensions in the order of tens of micrometres are presented. The ability to fabricate and structure thick functional films with embedded metal electrode structures offers the possibility to create novel micro-device structures suitable for use in micro-electromechanical systems (MEMS).     

Morphological properties of Ag₂SeTe nano thin films prepared by thermal evaporation

Semiconducting silver selenide telluride (Ag₂SeTe) thin films were prepared with different thicknesses onto glass substrates at room temperature using thermal evaporation technique. The structural properties were determined as a function of thickness by X‐ray diffraction exhibiting no preferential orientation along any plane; however, the films are found to have peaks corresponding to mixed phase. The morphology of these films was studied using scanning electron microscope and atomic force microscopy respectively, and is reported. The morphological properties are found to be very sensitive to the thin film thickness. The composition of the films is also estimated using energy dispersive analysis using X‐rays and are also reported.